Aluminum → Melphalan

HRID 1972145Notes

Reaction equation

HRID 1972145 reaction equation
[CH:1]1[C:6]([CH2:7][C@H:8]([NH2:12])[C:9]([OH:11])=[O:10])=[CH:5][CH:4]=[C:3]([N:13]([CH2:17][CH2:18][Cl:19])[CH2:14][CH2:15][Cl:16])[CH:2]=1.Cl.[Al]>O>[CH:1]1[C:6]([CH2:7][C@H:8]([NH2:12])[C:9]([OH:11])=[O:10])=[CH:5][CH:4]=[C:3]([N:13]([CH2:14][CH2:15][Cl:16])[CH2:17][CH2:18][Cl:19])[CH:2]=1

Participants

5

Reactant 2

HCID 5359268AluminumHCID 9927978Melphalan hydrochloride

Product 1

HCID 460612MelphalanYield 96%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 178435178HCID 178435178, compoundSolvent

Procedure

Place 200˜1000 g of Melphalan HCl (IM1036) into the vacuum flask, and quickly mount the vacuum flask to a Lyophilizer with the pressure preset at 225 mmHg and temperature at <−40° C. The freeze-drying process is continued overnight until the water content meets the specification requirement. The vacuum is released and the product is weighed. The product is packed in polypropylene bags inside a sealed aluminum pouch and stored at 2˜8° C. in a refrigerator, to protect it from light and moisture. The yield is 96˜99% of theoretical yield.

Workup

  1. customat <−40° C
  2. customstored at 2˜8° C. in a refrigerator

Sources & evidence

ORD record
ord-c50402d7c9d447338ee08f25d0ddb77e
Source dataset
uspto-grants-2013_04
Patent number
US08431735B2

Reaction notes

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