6-CHLORO-2-HEXANONE:-

Preparation of 2-methyl-5,6-dihydro-4H-pyran3-carboxylic acid methyl ester9. :--

To a solution of methyl acetoacetate 8 (10.0 g, 0.086 mole) in isopropyl alcohol (100 mL) was added
chlorobromopropane (13.5 g, 0.08 mole) and K2CO3 (14.24 g, 0.103 mole) and the reaction mixture
heated on a steam-bath at 80oC for 9 hr. The reaction was monitored by TLC. When the reaction was
complete, isopropyl alcohol was removed in vacuo, the residue was cooled to rt, diluted with water
and extracted with methylene chloride (2 50=100mL). The methylene chloride extract was washed
with water (150 mL) dried over Na2SO4 filtered, and concentrated to obtain a liquid which on
fractional distillation gave 9,yield 12.1 g (90%).

Preparation of 6-chloro-2-hexanone3.:--

A solution of pyran ester 9 (5 g, 0.03 mole) in concentrated HCl (20 mL) at 60oC was simultaneously
saturated with HCl gas. The reaction mixture was heated to 50oC for 3 hr. When the reaction was
complete, the mixture was cooled to rt, diluted with water, extracted with methylene chloride
(3×30=90 mL) and the combined layer distilled to obtain a residue. Purification of the crude residue
by fractional distillation gave a pure compound 3, yield 4 g (93%).
Rm cost Column1
Input Price
(rs)/kg
MEA 150
IPA 65
CBP 535
K2Co3 63
DMC 47
HCL 15
Na2So4 10
Total 885
DI AMINOBENZOPHENONE (DABP)

Charge water(150 Kg) & caustic lye(480kg) heat up to 80 to 85 c. After temp charge
sulphur(196Kg) and heat to 80 to 85 c.
Sparkler filter the solution .
Charge methanol(500 Kg) and NABP (200Kg) Reflux the solution until reaction complete
check by TLC.
Filter the solution with charcoal.
After filtration distill out MeOH(475 Kg).
After that crystallization of R.mass with water (200Kg).

Filter the solution . wet cake conversion 95%. Mother liquor(950 Kg).

Mass Balance

Input Kg Output Kg RM
Water 350 Product 301 Cost
Caustic /kg
lye 480 Rec. Methanol 475 Caustic 30
sulphur 196 ML 950 lye
sulphur 18
methanol 500
methanol 50
NABP 200
NABP 500
Total 1726 1726
Total 598
Ilaprazol intermediate : (2-Mercapto-5-Nitrobenzimidazole)

O-phenylenediamines (0.065 mol) was heated with N-aminorhodanine (0.065 mol) in xylen (50 ml) for 5 hours

. The obtained residue was filtered and was crystallized from aqueous alcohol (charcoal).

The obtained solid was recrystallized in ethanol.

Input Price/kg
O-
phenylenediamines 375
N-aminorhodanine 200
xylen 80
ethanol 100

Total cost 755

Methylcobalamine :
Prepare solution of cynocobalamine(13g) and cobalt chloride(ii)hexahydrate
(0.91g ) .
Add prepare solution in water (169 ml).
Heat at 35-37c.
Under nitrogen atmosphere solution of dimethyl carbonate(4.75 g) in methyl
ethyl ketone(13 ml). & solution of sodium borohydried(5.2 gm) in 26ml water
in 2N sodium hydroxide added in r.mass over period of 3 hr.
Maintain for 1 hr.(35 to 37)
Cool at 12c.
Stir for 3 hr.
Filter the solution.
Solid obtain was treated with 182 ml of aceton/water(50/50) at 35-40c.
Remove acetone at reduced pressure.
Aq solution is chromatgraphide through 500ml non polar resin. Inorganic salt
were remove by washing with water..
Eluting of methylcobalamine with a mixture of methanol/water(50/50).
Precipitation with 10ml acetone.

Input Price
(rs)/kg
cynocobalamine 9000
cobalt chloride(ii)hexahydrate 29
dimethyl carbonate 64
methyl ethyl ketone 110
sodium borohydried 1900
sodium hydroxide 50
methanol 50
Diaone hp20 2700
acetone 45
Total 13948
Cetrimide
Prepare solution of ethyl acetate(250l) and farmin dm4098.(210kg)

Stir the r.mass.

Purge methyl bromide gas in r.mass below 40.c. (Sodium bromide + di methyl sulphate)

Filter the solution.

Wash with ethyl acetate.

Input Price
(rs)/kg
ethyl acetate 55
Farmin DM4098 160
sodium bromide 150
DMS 45

Total 410