Ethanol → HCID 11978594、化合物

HRID 1851427ノート

反応式

HRID 1851427 の反応式
[C:1]([C:3]1[NH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[NH:12][S:13]([C:16]1[S:17][CH:18]=[CH:19][CH:20]=1)(=[O:15])=[O:14])#[N:2].N[CH2:22][CH2:23][SH:24].C(O)C>O>[S:24]1[CH2:23][CH2:22][N:2]=[C:1]1[C:3]1[NH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[NH:12][S:13]([C:16]1[S:17][CH:18]=[CH:19][CH:20]=1)(=[O:14])=[O:15]

参加物

5

反応物 3

HCID 702EthanolHCID 6058CysteamineHCID 57901755HCID 57901755、化合物

生成物 1

HCID 11978594HCID 11978594、化合物収率 29.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

A mixture of N-(2-cyano-1H-indol-7-yl)thiophene-2-sulfonamide (0.54 g), 2-aminoethanethiol (0.14 g) and ethanol (20 mL) was stirred at 60° C. overnight. Water was added to the reaction mixture, and the obtained crystals were filtrated, washed with water and dried. The obtained crystals were subjected to silica gel column chromatography, and eluted with ethyl acetate. The eluate was treated with activated carbon and concentrated to give the title compound (0.19 g, yield 29%) as colorless crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point 189-190° C.

後処理

  1. filtrationthe obtained crystals were filtrated
  2. washwashed with water
  3. customdried
  4. washeluted with ethyl acetate
  5. additionThe eluate was treated with activated carbon
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-2b76a62c22b84eea8cf4a66740f73062
出典データセット
uspto-grants-2015_02
特許番号
US08957070B2

反応ノート

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