Potassium Carbonate → HCID 178424319、化合物

HRID 497119

反応式

HRID 497119 の反応式
[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[C:4](=[O:21])[N:5]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:20])[C:6]([CH2:12]Cl)=[N:7]2.O.[N:23]1[C:31](=[S:32])[C:30]2[NH:29][CH:28]=[N:27][C:26]=2[NH:25][CH:24]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[C:4](=[O:21])[N:5]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:20])[C:6]([CH2:12][S:32][C:31]1[N:23]=[CH:24][N:25]=[C:26]3[C:30]=1[N:29]=[CH:28][NH:27]3)=[N:7]2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27243506-Mercaptopurine MonohydrateHCID 124873735-Chloro-2-chloromethyl-3-o-tolyl-3H-quinazolin-4-one

生成物 1

HCID 178424319HCID 178424319、化合物収率 52.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Prepared according to Procedure C using Intermediate 2j (200 mg, 0.626 mmol), 6-kinases -mercaptopurine monohydrate (93 mg, 0.546 mmol), K2CO3 (95 mg, 0.689 mmol), and DMF (4 mL). The crude product was recrystallized from EtOH to provide 125 mg of an off-white solid (46%), mp 213.9° C. 1H NMR (DMSO-d6) δ: 13.53 (br s, 1H); 8.49 (s, 1H); 8.44 (s, 1H); 7.78 (t, J=7.9 Hz, 1H); 7.63 (d, J=8.2 Hz, 1H); 7.59 (d, J=7.7 Hz, 1H); 7.49 (d, J=6.9 Hz, 1H); 7.24-7.41 (m, 3H); 4.32-4.45 (m, 2H); 2.14 (s, 3H). 13C NMR (DMSO-d6) ppm: 158.9, 157.2, 154.2, 151.5, 149.7, 149.6, 143.5, 136.1, 135.9, 135.1, 133.2, 131.3, 130.3, 130.0, 129.9, 129.1, 127.6, 127.1, 117.8, 32.4, 17.5. MS (ES): m/z 438.0 (M+). Anal. calcd. for C21H15ClN6OS: C, 58.00; H, 3.48; Cl, 8.15; N, 19.32; S, 7.37. Found: C, 58.05; H, 3.38; Cl, 8.89; N, 18.38; S, 7.00.

後処理

  1. customPrepared
  2. customThe crude product was recrystallized from EtOH

出典と根拠

ORDレコード
ord-94c7546ad9174c34b957506310d3e1d7
出典データセット
uspto-grants-2005_09
特許番号
US06949535B2

関連ノート

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