HCID 86614812、化合物 → HCID 86614818、化合物

HRID 1686157ノート

反応式

HRID 1686157 の反応式
[CH3:1][C:2]1[C:10]([CH3:19])([CH2:11][CH2:12][CH2:13][CH2:14][S:15]([O-:18])(=[O:17])=[O:16])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([S:20]([O-:23])(=[O:22])=[O:21])[CH:8]=2)[N:3]=1.[Na+:24].[Na+]>C1COS(=O)(=O)CC1>[CH3:1][C:2]1[C:10]([CH3:19])([CH2:11][CH2:12][CH2:13][CH2:14][S:15]([O-:18])(=[O:16])=[O:17])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([S:20]([O-:23])(=[O:21])=[O:22])[CH:8]=2)[N+:3]=1[CH2:11][CH2:12][CH2:13][CH2:14][S:15]([O-:18])(=[O:17])=[O:16].[Na+:24].[Na+:24]

参加物

3

反応物 1

HCID 86614812HCID 86614812、化合物

生成物 1

HCID 86614818HCID 86614818、化合物収率 217.1%

試薬・触媒・溶媒 1

HCID 154111,4-Butane sultone溶媒

反応条件

温度
150 °C

実験手順

Disodium 2,3-dimethyl-3-(4-sulphonatobutyl)-3H-indole-5-sulphonate (1.0 g) and 1,4-butanesultone (10 ml) were mixed and heated under nitrogen at 150° C. for 52 hrs to give a dark purple slurry. After cooling, the mixture was triturated with ethyl acetate: the solid portion was collected by filtration, washed with ethyl acetate and diethyl ether, then dried under high vacuum over phosphorus pentoxide to give the title product (1.45 g), which was used directly without purification.

後処理

  1. customto give a dark purple slurry
  2. temperatureAfter cooling
  3. customthe mixture was triturated with ethyl acetate
  4. filtrationthe solid portion was collected by filtration
  5. washwashed with ethyl acetate and diethyl ether
  6. dry with materialdried under high vacuum over phosphorus pentoxide

出典と根拠

ORDレコード
ord-b865b0f68dc94353ac068be4a51a97f3
出典データセット
uspto-grants-2012_04
特許番号
US08148539B2

反応ノート

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