Trifluoroacetic acid → 1-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane

HRID 1434567노트

반응식

HRID 1434567 반응식
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][CH2:25][N:26]3[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)=[CH:18][CH:17]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[N:26]1([CH2:25][CH2:24][CH2:23][O:22][C:19]2[CH:20]=[CH:21][C:16]([CH2:15][N:11]3[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]3)=[CH:17][CH:18]=2)[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 102964254-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane-1-carboxylic acid tert-butyl ester

생성물 1

HCID 596405921-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane수율 89.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane-1-carboxylic acid tert-butyl ester (D3) (2.27 g, 5.27 mmol) was dissolved in dichloromethane (10 ml), treated with trifluoroacetic acid (5 ml) and stirred at room temperature under argon for 2 hours. The solvent was removed in vacuo and the residue dissolved in methanol and passed down an SCX column (10 g) eluting with methanol followed by 0.88 ammonia/methanol (1:9). The basic fractions were combined and concentrated in vacuo to afford the title compound (1.57 g).

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in methanol
  3. washeluting with methanol
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-143a97be32394813984dc4f3a46bc604
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07615550B2

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