Benzenesulfonyl chloride, 3,4-dichloro- → tert-Butyl trans-6-[(3,4-dichlorophenyl)sulfonyl]-6,7,7a,8,10,10a-hexahydropyrido[3,2-c]pyrrolo[3,4-e]azepine-9(5H)-carboxylate

HRID 84967

반응식

HRID 84967 반응식
[N:1]1[C:11]2[C@@H:10]3[CH2:12][N:13]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:14][C@H:9]3[CH2:8][NH:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[Cl:29][C:30]1[CH:31]=[C:32]([S:37](Cl)(=[O:39])=[O:38])[CH:33]=[CH:34][C:35]=1[Cl:36].[OH-].[Na+]>ClCCl>[Cl:29][C:30]1[CH:31]=[C:32]([S:37]([N:7]2[CH2:8][C@@H:9]3[CH2:14][N:13]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:12][C@H:10]3[C:11]3[N:1]=[CH:2][CH:3]=[CH:4][C:5]=3[CH2:6]2)(=[O:38])=[O:39])[CH:33]=[CH:34][C:35]=1[Cl:36]

참가 물질

6

반응물 4

HCID 7383Benzenesulfonyl chloride, 3,4-dichloro-HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 123947677tert-Butyl trans-6,7,7a,8,10,10a-hexahydropyrido[3,2-c]pyrrolo[3,4-e]azepine-9(5H)-carboxylate

생성물 1

HCID 123445055tert-Butyl trans-6-[(3,4-dichlorophenyl)sulfonyl]-6,7,7a,8,10,10a-hexahydropyrido[3,2-c]pyrrolo[3,4-e]azepine-9(5H)-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of Example 334B (100 mg, 0.34 mmol) and triethylamine (0.097 mL, 0.69 mmol) in dichloromethane (2 mL) was stirred at ambient temperature for 10 minutes. 3,4-Dichlorobenzene-1-sulfonyl chloride (0.52 mmol, 1.5 equivalents) was added, and the reaction mixture was stirred at room temperature overnight. A 10% NaOH solution (2 mL) was added; the dichloromethane layer was separated, treated with water (2 mL) and dried over Na2SO4. The solvent was removed in vacuo to give the title compound.

후처리

  1. customthe dichloromethane layer was separated
  2. additiontreated with water (2 mL)
  3. dry with materialdried over Na2SO4
  4. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-f6e17a941eae4d229020d7b4426a778f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846951B2

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