Water → 1-benzylazetidine-3,3-dicarboxylic Acid

HRID 1722480

반응식

HRID 1722480 반응식
BrBr.[CH2:3]([N:10]1[CH2:13][C:12]([CH2:16][OH:17])([CH2:14][OH:15])[CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[OH-:18].[Na+].[OH2:20]>S([O-])([O-])(=O)=O.[Ni+2]>[CH2:3]([N:10]1[CH2:13][C:12]([C:14]([OH:20])=[O:15])([C:16]([OH:18])=[O:17])[CH2:11]1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24408BromineHCID 20164320[1-Benzyl-3-(hydroxymethyl)azetidin-3-YL]methanol

생성물 1

HCID 113108851-benzylazetidine-3,3-dicarboxylic Acid

시약·촉매·용매 1

HCID 24586Nickel Sulfate촉매

실험 절차

Bromine (10.6 g) was slowly added at 20° C. over 8 hours to a mixture of N-benzyl-3,3-bis(hydroxymethyl)azetidine (2.1 g) in water (50 ml) containing sodium hydroxide (9.3 g) and nickel chloride 6.0 aq. (1.5 g). After stirring overnight, the green precipitate of nickel hydroxide was filtered off, and the filtrate evaporated to dryness. The residue was boiled in ethanol, and the insoluble material (desired product as sodium salt and sodium bromide) separated and worked up to yield the N-benzyl-azetidine-3,3-dicarboxylic acid.

후처리

  1. filtrationthe green precipitate of nickel hydroxide was filtered off
  2. customthe filtrate evaporated to dryness
  3. customthe insoluble material (desired product as sodium salt and sodium bromide) separated

출처 및 근거

ORD 기록
ord-2c659e65c5bc4e558fb6affc643a49c5
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04855452

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