Triethylamine → 4-[N'-Methyl-N'-(3,5-bistrifluoromethyl-benzoyl)-amino]-5-(naphth-2-yl)-pentanoic acid N-propyl-N-phenyl-amide

HRID 583417

반응식

HRID 583417 반응식
[CH3:1][N:2]([CH:19]([CH2:25][C:26]1[CH:35]=[CH:34][C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:27]=1)[CH2:20][CH2:21][C:22](O)=[O:23])[C:3](=[O:18])[C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[C:6]([C:14]([F:17])([F:16])[F:15])[CH:5]=1.[CH2:36]([NH:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)[CH2:37][CH3:38].C(N(CC)CC)C.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[CH2:36]([N:39]([C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)[C:22](=[O:23])[CH2:21][CH2:20][CH:19]([N:2]([CH3:1])[C:3](=[O:18])[C:4]1[CH:5]=[C:6]([C:14]([F:16])([F:17])[F:15])[CH:7]=[C:8]([C:10]([F:12])([F:13])[F:11])[CH:9]=1)[CH2:25][C:26]1[CH:35]=[CH:34][C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:27]=1)[CH2:37][CH3:38]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 12153Benzenamine, N-propyl-HCID 213105294-[N-Methyl-N-(3,5-bistrifluoromethyl-benzoyl)-amino]-5-(naphth-2-yl)-pentanoic acid

생성물 1

HCID 867543264-[N'-Methyl-N'-(3,5-bistrifluoromethyl-benzoyl)-amino]-5-(naphth-2-yl)-pentanoic acid N-propyl-N-phenyl-amide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture consisting of 100 mg of 4-[N-methyl-N-(3,5-bistrifluoromethyl-benzoyl)-amino]-5-(naphth-2-yl)-pentanoic acid, 29.9 mg of N-propyl-aniline, 85.3 mg of propanephosphonic acid anhydride, 154 νl of triethylamine and 2 ml of methylene chloride is left to stand at room temperature for 18 hours. 0.5 ml of 1N potassium carbonate solution is then added and the mixture is shaken vigorously. After separation of the phases, the organic phase is separated off and concentrated by evaporation. Chromatography of the residue over silica gel with methylene chloride/methanol 19:1 yields the title compound in the form of a yellow foam. Rf value=0.63 (methylene chloride/methanol 19:1).

후처리

  1. waitis left
  2. customAfter separation of the phases
  3. customthe organic phase is separated off
  4. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-9a099cbfe32d42a4b9f05ae2dcf3400c
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929067

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