Sodium Hydroxide → 4-[N-(2-Benzyloxy-5-bromobenzyl)aminomethyl]Benzoic Acid

HRID 1005996노트

반응식

HRID 1005996 반응식
[CH2:1]([O:8][C:9]1[CH:28]=[CH:27][C:26]([Br:29])=[CH:25][C:10]=1[CH2:11][NH:12][CH2:13][C:14]1[CH:24]=[CH:23][C:17]([C:18]([O:20]CC)=[O:19])=[CH:16][CH:15]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CO>[CH2:1]([O:8][C:9]1[CH:28]=[CH:27][C:26]([Br:29])=[CH:25][C:10]=1[CH2:11][NH:12][CH2:13][C:14]1[CH:24]=[CH:23][C:17]([C:18]([OH:20])=[O:19])=[CH:16][CH:15]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22675503ethyl 4-[N-(2-benzyloxy-5-bromobenzyl)aminomethyl]benzoate

생성물 1

HCID 47205174-[N-(2-Benzyloxy-5-bromobenzyl)aminomethyl]Benzoic Acid수율 60.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a mixture of ethyl 4-[N-(2-benzyloxy-5-bromobenzyl)-aminomethyl]benzoate (1.4 g) in methanol (25 ml) was added 2N sodium hydroxide solution (7.7 ml). The mixture was heated at reflux for 30 minutes, left to stand for 2 hours at ambient temperature, the solvent evaporated and the residue mixed with water (20 ml). The mixture was acidified with acetic acid, the precipitate filtered off and crystallised form ethyl acetate to give the title compound (800 mg) mpt 209° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 30 minutes
  3. waitleft
  4. customthe solvent evaporated
  5. additionthe residue mixed with water (20 ml)
  6. filtrationthe precipitate filtered off
  7. customcrystallised
  8. customform ethyl acetate

출처 및 근거

ORD 기록
ord-9b9cfa63525041f2a39fb741bcedd64a
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787562B2

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