Triethylamine → 1-(1-(2,4-Dimethoxybenzoyl)-4-piperidyl)indol-2-one

HRID 1377688노트

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HRID 1377688 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][C:8]2=[O:16])[CH2:3][CH2:2]1.[CH3:17][O:18][C:19]1[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:20]=1[C:21](Cl)=[O:22].C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH3:17][O:18][C:19]1[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:20]=1[C:21]([N:1]1[CH2:6][CH2:5][CH:4]([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][C:8]2=[O:16])[CH2:3][CH2:2]1)=[O:22]

참가 물질

5

반응물 3

HCID 8471Triethylamine2회HCID 27347192,4-Dimethoxybenzoyl chlorideHCID 27611521-Piperidin-4-yl-1,3-dihydro-2H-indol-2-one

생성물 1

HCID 229146571-(1-(2,4-Dimethoxybenzoyl)-4-piperidyl)indol-2-one수율 45.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
0 °C

실험 절차

1-(4-Piperidyl)indol-2-one (53 mg, 0.245 mmole), 2,4-dimethoxybenzoyl chloride (54 mg, 0.27 mmole), and 38 mL (0.27 mmole) triethylamine were mixed in 4 ml of chloroform at 0° C. The reaction mixture was stirred at 0° C. for 5 minutes and then at 23° C. for 15 minutes during which time the pH was adjusted to 7.5 with triethylamine. The reaction mixture was concentrated under reduced pressure and the residue was purified by preparative thick layer chromatography (CHCl3 --CH3OH--NH4OH; 95:5:0.5) to yield 42 mg of the title compound: m.p. 88°-93° C.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by preparative thick layer chromatography (CHCl3 --CH3OH--NH4OH; 95:5:0.5)

출처 및 근거

ORD 기록
ord-75a0481253b94f3ea3f76576417ad1fe
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05665719

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