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Water → (2R)-4-benzyl-2-[4-chloro-3-(tert-butyldimethylsilyloxy)benzyl]piperazine

HRID 1374997
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반응식

HRID 1374997 반응식
[Cl:1][C:2]1[CH:21]=[CH:20][C:5]([CH2:6][C@@H:7]2[CH2:12][N:11]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:10][CH2:9][NH:8]2)=[CH:4][C:3]=1[OH:22].C(N(CC)CC)C.[Si:30](Cl)([C:33]([CH3:36])([CH3:35])[CH3:34])([CH3:32])[CH3:31].O>ClCCl.CN(C)C1C=CN=CC=1>[CH2:13]([N:11]1[CH2:10][CH2:9][NH:8][C@H:7]([CH2:6][C:5]2[CH:20]=[CH:21][C:2]([Cl:1])=[C:3]([O:22][Si:30]([C:33]([CH3:36])([CH3:35])[CH3:34])([CH3:32])[CH3:31])[CH:4]=2)[CH2:12]1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 28928tert-Butyldimethylsilyl chlorideHCID 54261549(2R)-2-(4-chloro-3-hydroxybenzyl)-4-benzylpiperazine

생성물 1

HCID 54436042(2R)-4-benzyl-2-[4-chloro-3-(tert-butyldimethylsilyloxy)benzyl]piperazine수율 79.9%

시약·촉매·용매 2

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 6344Dichloromethane용매

실험 절차

To a solution of (2R)-2-(4-chloro-3-hydroxybenzyl)-4-benzylpiperazine (3.78 g) and triethylamine (5.71 ml) in dichloromethane was added 4-dimethylaminopyridine (0.29 g) and tert-butyldimethylsilyl chloride (5.30 g) successively with ice bath cooling under nitrogen atmosphere. After stirring overnight at room temperature, water (50 ml) was added to the mixture and the organic layer was separated, washed with brine, dried over sodium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel with a mixture of dichloromethane and methanol (10:1) as eluent to give (2R)-4-benzyl-2-[4-chloro-3-(tert-butyldimethylsilyloxy)benzyl]piperazine (4.11 g) as an oil.

후처리

  1. temperaturecooling under nitrogen atmosphere
  2. customthe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo
  6. customThe residue was purified by column chromatography on silica gel with a mixture of dichloromethane and methanol (10:1) as eluent

출처 및 근거

ORD 기록
ord-fb3029d8fe83458faaac2560f2980618
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07166598B2

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