Cyclohexylamine → HCID 58382222、化合物

HRID 1628018ノート

反応式

HRID 1628018 の反応式
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:5]=[C:4]2[N:13]([Si](C(C)C)(C(C)C)C(C)C)[CH:14]=[CH:15][C:3]=12.[CH:26]1([NH2:32])[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]1>>[CH2:11]([O:10][C:8]([C:7]1[C:2]([NH:32][CH:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)=[C:3]2[CH:15]=[CH:14][NH:13][C:4]2=[N:5][CH:6]=1)=[O:9])[CH3:12]

参加物

3

反応物 2

HCID 7965CyclohexylamineHCID 58382073HCID 58382073、化合物

生成物 1

HCID 58382222HCID 58382222、化合物収率 48.2%

反応条件

温度
80 °C

実験手順

A mixture of ethyl 4-chloro-1-(triisopropylsilyl)-1H-pyrrolo[2,3-b]pyridine-5-carboxylate (1.5 g, 3.9 mmol) and cyclohexylamine (2.34 g, 23.6 mmol) was stirred at about 80° C. for about 24 h. The solvent was removed under reduced pressure. The residue was suspended in Et2O and the precipitate was collected by filtration and dried under vacuum. The solid was washed with water and dried under vacuum again to give ethyl-4-(cyclohexylamino)-1H-pyrrolo[2,3-b]pyridine-5-carboxylate (0.54 g, 48%): LC/MS (Table 2, Method b) Rt=2.56 min.; MS m/z: 288 (M+H)+.

後処理

  1. customThe solvent was removed under reduced pressure
  2. filtrationthe precipitate was collected by filtration
  3. customdried under vacuum
  4. washThe solid was washed with water
  5. customdried under vacuum again

出典と根拠

ORDレコード
ord-e29aa407bd574a2fa11ef5049ccafbc9
出典データセット
uspto-grants-2014_07
特許番号
US08785639B2

反応ノート

読み込み中…