Pyridine → HCID 21876712、化合物

HRID 723787ノート

反応式

HRID 723787 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH2:14][CH2:13][S:12][CH2:11][CH:10]=2)=[C:4]([F:15])[CH:3]=1.N1C=CC=CC=1.Cl[C:23]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:24]>ClCCl>[CH2:26]([O:25][C:23]([NH:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH2:14][CH2:13][S:12][CH2:11][CH:10]=2)=[C:4]([F:15])[CH:3]=1)=[O:24])[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 10387Benzyl chloroformateHCID 21876582HCID 21876582、化合物

生成物 1

HCID 21876712HCID 21876712、化合物収率 94.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

4-(4-Amino-2,6-difluorophenyl)-5,6-dihydro-2H-thiopyran (15.0 g, 66 mM) was dissolved in dry dichloromethane (250 ml), pyridine (9.45 g, 113 mM) added, and the whole stirred under nitrogen at −20°. Benzyl chloroformate (17.1 g, 100 mM) in dry dichloromethane (25 ml) was added dropwise, and the mixture allowed to warm to ambient over 18 hours. The mixture was washed with hydrochloric acid (1M, 2×200 ml), then brine (200 ml) and dried (magnesium sulfate). Evaporation to a small volume and dilution with isohexane gave the desired product as a white solid (22.5 g).

後処理

  1. temperatureto warm
  2. washThe mixture was washed with hydrochloric acid (1M, 2×200 ml)
  3. dry with materialbrine (200 ml) and dried (magnesium sulfate)
  4. customEvaporation to a small volume and dilution with isohexane

出典と根拠

ORDレコード
ord-f2a168d2dbd54af38e3d5340812cfd30
出典データセット
uspto-grants-2006_11
特許番号
US07141583B2

反応ノート

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