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Ammonia → Bisindolylmaleimide X hydrochloride

HRID 863667
ノート
印刷プレビュー

反応式

HRID 863667 の反応式
FC(F)(F)S(OS(C(F)(F)F)(=O)=O)(=O)=O.C(O[CH2:20][CH:21]1[CH2:50][CH2:49][N:24]2[C:25]3[C:30]([C:31]([C:32]4[C:33](=O)[O:34][C:35](=[O:47])[C:36]=4[C:37]4[C:45]5[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=5)[N:39]([CH3:46])[CH:38]=4)=[C:23]2[CH2:22]1)=[CH:29][CH:28]=[CH:27][CH:26]=3)(=O)C.[N:51]1C(C)=CC(C)=CC=1C.[NH3:60].[Cl:61]CCl>>[ClH:61].[NH2:60][CH2:20][CH:21]1[CH2:50][CH2:49][N:24]2[C:25]3[C:30]([C:31]([C:32]4[C:33](=[O:34])[NH:51][C:35](=[O:47])[C:36]=4[C:37]4[C:45]5[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=5)[N:39]([CH3:46])[CH:38]=4)=[C:23]2[CH2:22]1)=[CH:29][CH:28]=[CH:27][CH:26]=3
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 222AmmoniaHCID 6344Dichloromethane2 回HCID 79532,4,6-TrimethylpyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 103898823-[8-(Acetoxymethyl)-6,7,8,9-tetrahydropyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)furan-2,5-dione

生成物 1

HCID 11539879
Bisindolylmaleimide X hydrochloride

反応条件

温度
10 °C

実験手順

2.50 g of trifluoromethanesulfonic anhydride in 330 ml of dichloromethane were treated at 0° C. under a nitrogen atmosphere with a suspension of 1.87 g of the pyrroledione product of Example 1 and 0.94 g of collidine in 280 ml of dichloromethane. After 2.5 hours, the mixture was allowed to warm to 10° C. Then, 37 ml of 33% aqueous ammonia were added and the mixture was allowed to warm to room temperature overnight. The mixture was washed with water, dried and evaporated. The residue was subjected to chromatography on silica gel with dichloromethane/methanol/acetic acid/water (90:18:3:2). The combined product-containing fractions were treated with 2M hydrochloric acid and evaporated to give 930 mg of 3-[8-(aminomethyl)-6,7,8,9-tetrahydropyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione hydrochloride of melting point 310°-313° C.

後処理

  1. temperatureto warm to room temperature overnight
  2. washThe mixture was washed with water
  3. customdried
  4. customevaporated
  5. additionThe combined product-containing fractions
  6. additionwere treated with 2M hydrochloric acid
  7. customevaporated

出典と根拠

ORDレコード
ord-ec06762f6fcf445e954391d79354fb9a
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05721245

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート