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

反応式

HRID 84967 の反応式
[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]

参加物

6

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f6e17a941eae4d229020d7b4426a778f
出典データセット
uspto-grants-2014_09
特許番号
US08846951B2

関連ノート

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