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

HRID 1377688

反応式

HRID 1377688 の反応式
[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]

参加物

5

反応物 3

HCID 8471Triethylamine2 回HCID 27347192,4-Dimethoxybenzoyl chlorideHCID 27611521-Piperidin-4-yl-1,3-dihydro-2H-indol-2-one

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-75a0481253b94f3ea3f76576417ad1fe
出典データセット
uspto-grants-1997_09
特許番号
US05665719

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