Methanol → HCID 178474871、化合物

HRID 1373137ノート

反応式

HRID 1373137 の反応式
C([N:4]1[C:12]2[C:7](=[CH:8][C:9]([N:13](C(=O)C)[S:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)(=[O:16])=[O:15])=[CH:10][CH:11]=2)[C:6](=[C:26](OCC)[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:5]1=[O:36])(=O)C.[C:37]([N:40]([C:50]1[CH:56]=[CH:55][C:53]([NH2:54])=[CH:52][CH:51]=1)[CH2:41][CH2:42][NH:43]C(=O)C(F)(F)F)(=[O:39])[CH3:38].CO.[OH-].[Na+]>CN(C=O)C.O>[C:37]([N:40]([C:50]1[CH:51]=[CH:52][C:53]([NH:54]/[C:26](=[C:6]2\[C:5](=[O:36])[NH:4][C:12]3[C:7]\2=[CH:8][C:9]([NH:13][S:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)(=[O:16])=[O:15])=[CH:10][CH:11]=3)/[C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)=[CH:55][CH:56]=1)[CH2:41][CH2:42][NH2:43])(=[O:39])[CH3:38]

参加物

7

反応物 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 120470014-[N-acetyl-N-(2-trifluoroacetylamino-ethyl)-amino]-anilineHCID 695098291-acetyl-3-(1-ethoxy-1-phenyl-methylidene)-5-(N-acetyl-N-phenylsulphonyl-amino)-2-indolinone

生成物 1

HCID 178474871HCID 178474871、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 0.5 g (1 mmol) of 1-acetyl-3-(1-ethoxy-1-phenyl-methylidene)-5-(N-acetyl-N-phenylsulphonyl-amino)-2-indolinone and 0.3 g (1.2 mmol) of 4-[N-acetyl-N-(2-trifluoroacetylamino-ethyl)-amino]-aniline are stirred in 5 ml of DMF for 6 hours at 120° C. After cooling to ambient temperature 5 ml of methanol and 3 ml (6 mmol) of 2 N sodium hydroxide solution are added, and the mixture is stirred for 30 minutes. The reaction mixture is diluted with 50 ml of water and the crystalline precipitate is suction filtered and dried. The residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=9:1:0.1).

後処理

  1. additionare added
  2. filtrationfiltered
  3. customdried
  4. customThe residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=9:1:0.1)

出典と根拠

ORDレコード
ord-d7577033038f420bb8ac47a0ca3e5739
出典データセット
uspto-grants-2007_01
特許番号
US07160901B2

反応ノート

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