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

반응식

HRID 1167171 반응식
[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]

참가 물질

4

반응물 2

HCID 103412(5H)-Furanone2회HCID 15547168HCID 15547168, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d1917cadd3624a61b5a0a0bc90a13b33
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06617329B2

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