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Triethylamine → tert-Butyl 4-(thiophene-2-sulfonyl)piperazine-1-carboxylate

HRID 390978
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반응식

HRID 390978 반응식
[C:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N(CC)CC)C.[S:21]1[CH:25]=[CH:24][CH:23]=[C:22]1[S:26](Cl)(=[O:28])=[O:27]>C(Cl)Cl>[C:4]([O:3][C:1]([N:8]1[CH2:9][CH2:10][N:11]([S:26]([C:22]2[S:21][CH:25]=[CH:24][CH:23]=2)(=[O:28])=[O:27])[CH2:12][CH2:13]1)=[O:2])([CH3:7])([CH3:6])[CH3:5]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 855182-Thiophenesulfonyl chlorideHCID 143452tert-Butyl piperazine-1-carboxylate

생성물 1

HCID 17255579tert-Butyl 4-(thiophene-2-sulfonyl)piperazine-1-carboxylate수율 85%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To N-Boc-piperazine (500 mg) in DCM (10 ml) was added triethylamine (450 μl) and 2-thiophenesulfonyl chloride (530 mg). The reaction mixture was stirred at room temperature overnight, then partitioned between dichloromethane and water, washed with brine, organics were dried over MgSO4, filtered and volatiles removed in vacuo to give 4-(2-thiophenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester (759 mg).

후처리

  1. custompartitioned between dichloromethane and water
  2. washwashed with brine
  3. dry with materialorganics were dried over MgSO4
  4. filtrationfiltered
  5. customvolatiles removed in vacuo

출처 및 근거

ORD 기록
ord-384337ef22694ace9de4c6c1df1ead30
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383620B2

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