Diethylamine → N-ethylethanaminium 4-{1-[({1-[4-(trifluoromethyl)benzyl]-1H-indol-7-yl}carbonyl)amino]cyclopropyl}benzoate

HRID 1694385노트

반응식

HRID 1694385 반응식
[F:1][C:2]([F:35])([F:34])[C:3]1[CH:33]=[CH:32][C:6]([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][C:15]=3[C:17]([NH:19][C:20]3([C:23]4[CH:31]=[CH:30][C:26]([C:27]([OH:29])=[O:28])=[CH:25][CH:24]=4)[CH2:22][CH2:21]3)=[O:18])[CH:10]=[CH:9]2)=[CH:5][CH:4]=1.[CH2:36]([NH:38][CH2:39][CH3:40])[CH3:37].COC(C)(C)C>C(O)C>[F:35][C:2]([F:1])([F:34])[C:3]1[CH:33]=[CH:32][C:6]([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][C:15]=3[C:17]([NH:19][C:20]3([C:23]4[CH:24]=[CH:25][C:26]([C:27]([O-:29])=[O:28])=[CH:30][CH:31]=4)[CH2:21][CH2:22]3)=[O:18])[CH:10]=[CH:9]2)=[CH:5][CH:4]=1.[CH2:36]([NH2+:38][CH2:39][CH3:40])[CH3:37]

참가 물질

5

반응물 3

HCID 8021DiethylamineHCID 15413tert-Butyl methyl etherHCID 250030754-(1-(1-(4-(trifluoromethyl)benzyl)-1H-indole-7-carboxamido)cyclopropyl)benzoic acid

생성물 1

HCID 67279731N-ethylethanaminium 4-{1-[({1-[4-(trifluoromethyl)benzyl]-1H-indol-7-yl}carbonyl)amino]cyclopropyl}benzoate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-{1-[({1-[4-(trifluoromethyl)benzyl]-1H-indol-7-yl}carbonyl)amino]cyclopropyl}benzoic acid (13 g, 27.2 mmol) was dissolved in 146 ml ethanol. Diethylamine (3.4 ml, 33 mmol) was added and the mixture was stirred 30 min (formation of precipitate observed). 260 ml of methyl tert-butylether was added and the mixture aged one hour. The solid was collected by filtration, washed with methyl tert-butylether and dried under vacuum at 85° C. for 24 h. 1H NMR 6 Acetone-d6: 8.30 (1H, s), 7.90 (2H, d), 7.80 (1H, d), 7.55 (2H, d), 7.45-7.35 (4H, m), 7.15 (1H, d), 7.00 (2H, d), 6.70 (1H, d), 5.80 (2H, s), 2.60 (4H, q), 1.25-1.20 (2H, m), 1.10-1.05 (8H, m).

후처리

  1. customthe mixture aged one hour
  2. filtrationThe solid was collected by filtration
  3. washwashed with methyl tert-butylether
  4. customdried under vacuum at 85° C. for 24 h

출처 및 근거

ORD 기록
ord-99f274b087ce41579f6c2661aa68c990
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158671B2

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