Pyridine → 1-[7-(2,3-Dihydro-indole-1-sulfonyl)-3,4-dihydro-1H-isoquinolin-2-yl]-ethanone

HRID 22820

反応式

HRID 22820 の反応式
N1C=CC=CC=1.[C:7]([N:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][C:14]([S:20](Cl)(=[O:22])=[O:21])=[CH:15][CH:16]=2)[CH2:11]1)(=[O:9])[CH3:8].[NH:24]1[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH2:26][CH2:25]1>ClCCCl>[N:24]1([S:20]([C:14]2[CH:13]=[C:12]3[C:17]([CH2:18][CH2:19][N:10]([C:7](=[O:9])[CH3:8])[CH2:11]3)=[CH:16][CH:15]=2)(=[O:22])=[O:21])[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH2:26][CH2:25]1

参加物

5

反応物 3

HCID 1049PyridineHCID 10328IndolineHCID 126069042-Acetyl-1,2,3,4-tetrahydroisoquinoline-7-sulfonyl chloride

生成物 1

HCID 225920191-[7-(2,3-Dihydro-indole-1-sulfonyl)-3,4-dihydro-1H-isoquinolin-2-yl]-ethanone収率 67%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

Pyridine (0.85 ml, 10.5 mmol) was added to a stirred solution of 2-acetyl-1,2,3,4-tetrahydroisoquinoline-7-sulfonyl chloride (0.96 g, 3.5 mmol) and 2,3-dihydro-1H-indole (0.42 g, 3.5 mmol) in 1,2-dichlorethane (40 ml) at room temperature. After 3 h, the solution was washed with water (40 ml), dried (MgSO4) and concentrated in vacuo to an oil. The oil was purified by column chromatography over silica gel eluting with a gradient of dichloromethane/methanol to afford the title compound (D5) as an oil (0.83 g, 67%), MS: m/z (MH+) 357.

後処理

  1. washthe solution was washed with water (40 ml)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo to an oil
  4. customThe oil was purified by column chromatography over silica gel eluting with a gradient of dichloromethane/methanol

出典と根拠

ORDレコード
ord-7cd696d750fc4bb188418451dc6d5112
出典データセット
uspto-grants-2005_02
特許番号
US06849644B2

関連ノート

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