Water → HCID 58980117、化合物

HRID 28853

反応式

HRID 28853 の反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]3[NH:14][CH:15]=[CH:16][C:9]=23)[C:5]([C:17]2[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=2)=[N:4]1)[CH3:2].N1C=CC=CC=1.[CH:30]([N:33]=[C:34]=[O:35])([CH3:32])[CH3:31].O>ClCCl>[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]3[NH:14][CH:15]=[CH:16][C:9]=23)[C:5]([C:17]2[CH:23]=[CH:22][C:20]([NH:21][C:34]([NH:33][CH:30]([CH3:32])[CH3:31])=[O:35])=[CH:19][CH:18]=2)=[N:4]1)[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 61277Isopropyl isocyanateHCID 689998134-[1-ethyl-4-(1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-3-yl]aniline

生成物 1

HCID 58980117HCID 58980117、化合物収率 45%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 4-[1-ethyl-4-(1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-3-yl]aniline (0.19 mmol) in dichloromethane (1 mL) was treated with pyridine (0.39 mmol) and isopropyl isocyanate (0.39 mmol). The reaction mixture was stirred for 18 h at room temperature and poured into water (1 mL), followed by extraction with (3×3 mL) ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated in vacuo. Purification of the residue by Gilson reverse phase HPLC provided the title product as a white powder (45%). ESMS [M+H]+: 389.2

後処理

  1. extractionfollowed by extraction with (3×3 mL) ethyl acetate
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customPurification of the residue by Gilson reverse phase HPLC

出典と根拠

ORDレコード
ord-1beb9e6f6a7546959165bcc9db517abb
出典データセット
uspto-grants-2008_09
特許番号
US07419988B2

関連ノート

読み込み中…