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Benzyl chloroformate → HCID 54373813, 화합물

HRID 2106516
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HRID 2106516 반응식
Cl[C:2]([O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:3].[NH:12]1[CH2:17][CH2:16][CH:15]([N:18]2[CH2:23][CH2:22][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:20][CH2:19]2)[CH2:14][CH2:13]1.C(N(C(C)C)C(C)C)C>C(Cl)Cl>[CH2:5]([O:4][C:2]([N:12]1[CH2:17][CH2:16][CH:15]([N:18]2[CH2:19][CH2:20][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:22][CH2:23]2)[CH2:14][CH2:13]1)=[O:3])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10387Benzyl chloroformateHCID 81531DiisopropylethylamineHCID 17750356tert-Butyl 4-(piperidin-4-yl)piperazine-1-carboxylate

생성물 1

HCID 54373813HCID 54373813, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 7.18 mL (48.0 mmol) benzyl chloroformate in 50 mL DCM was added dropwise to 12.3 g (45.7 mmol) tert-butyl 4-piperidin-4-yl-piperazine-1-carboxylate and 8.2 mL (50 mmol) N-ethyldiisopropylamine in 200 mL DCM while cooling with ice and the reaction mixture was stirred overnight at RT. It was washed with 200 mL of 15% K2CO3 solution, the organic phase was separated off and dried over Na2SO4. After elimination of the desiccant and solvent the residue was further reacted without any further purification.

후처리

  1. temperaturewhile cooling with ice
  2. washIt was washed with 200 mL of 15% K2CO3 solution
  3. customthe organic phase was separated off
  4. dry with materialdried over Na2SO4
  5. customAfter elimination of the desiccant and solvent the residue was further reacted without any further purification

출처 및 근거

ORD 기록
ord-a1d1f6e15d694e61995ae8a7c8f93941
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07579341B2

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