Cyclohexylamine → HCID 58382222, 화합물

HRID 1628018노트

반응식

HRID 1628018 반응식
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]

참가 물질

3

반응물 2

HCID 7965CyclohexylamineHCID 58382073HCID 58382073, 화합물

생성물 1

HCID 58382222HCID 58382222, 화합물수율 48.2%

반응 조건

온도
80 °C

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-e29aa407bd574a2fa11ef5049ccafbc9
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785639B2

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