2(5H)-Furanone → 4-[(3-Chloro-4-fluorophenyl)amino]-6-cyclopentylmethoxy-7-{2-[4-(2-oxo-tetrahydrofuran-4-yl)-piperazin-1-yl]-ethoxy}-quinazoline

HRID 1167171

反応式

HRID 1167171 の反応式
[O:1]1[CH2:5][CH:4]=[CH:3][C:2]1=[O:6].[Cl:7][C:8]1[CH:9]=[C:10]([NH:15][C:16]2[C:25]3[C:20](=[CH:21][C:22]([O:33][CH2:34][CH2:35][N:36]4[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]4)=[C:23]([O:26][CH2:27][CH:28]4[CH2:32][CH2:31][CH2:30][CH2:29]4)[CH:24]=3)[N:19]=[CH:18][N:17]=2)[CH:11]=[CH:12][C:13]=1[F:14]>CO>[Cl:7][C:8]1[CH:9]=[C:10]([NH:15][C:16]2[C:25]3[C:20](=[CH:21][C:22]([O:33][CH2:34][CH2:35][N:36]4[CH2:37][CH2:38][N:39]([CH:4]5[CH2:5][O:1][C:2](=[O:6])[CH2:3]5)[CH2:40][CH2:41]4)=[C:23]([O:26][CH2:27][CH:28]4[CH2:29][CH2:30][CH2:31][CH2:32]4)[CH:24]=3)[N:19]=[CH:18][N:17]=2)[CH:11]=[CH:12][C:13]=1[F:14]

参加物

4

反応物 2

HCID 103412(5H)-Furanone2 回HCID 15547168HCID 15547168、化合物

生成物 1

HCID 101672114-[(3-Chloro-4-fluorophenyl)amino]-6-cyclopentylmethoxy-7-{2-[4-(2-oxo-tetrahydrofuran-4-yl)-piperazin-1-yl]-ethoxy}-quinazoline

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

46 mg of (5H)-furan-2-one are added to a solution of 230 mg of 4-[(3-chloro-4-fluorophenyl)amino]-6-cyclopentylmethoxy-7-[2-(piperazin-1-yl)-ethoxy]-quinazoline in 2 ml of methanol. The reaction mixture is stirred for 24 hours at ambient temperature, then for another six at 50° C. In total, six more drops of (5H)-furan-2-one are added until the reaction is complete. The solvent is distilled off using the rotary evaporator and the crude product is purified by chromatography over an Alox column (activity stage III) with methylene chloride/methanol (98:2) as eluant. The desired product is obtained as a colourless solid.

後処理

  1. customat 50° C
  2. distillationThe solvent is distilled off
  3. customthe rotary evaporator
  4. customthe crude product is purified by chromatography over an Alox column (activity stage III) with methylene chloride/methanol (98:2) as eluant

出典と根拠

ORDレコード
ord-d1917cadd3624a61b5a0a0bc90a13b33
出典データセット
uspto-grants-2003_09
特許番号
US06617329B2

関連ノート

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