Water → 6-Benzoyl-3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine

HRID 1734045

반응식

HRID 1734045 반응식
[F:1][C:2]1[CH:28]=[CH:27][C:5]2[C:6]([CH:9]3[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][C:17]4[C:25]5[CH2:24][CH2:23][NH:22][CH2:21][C:20]=5[S:19][C:18]=4[CH3:26])[CH2:11][CH2:10]3)=[N:7][O:8][C:4]=2[CH:3]=1.[C:29](Cl)(=[O:36])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.O>C(N(CC)CC)C.C(Cl)(Cl)Cl>[C:29]([N:22]1[CH2:23][CH2:24][C:25]2[C:17]([CH2:16][CH2:15][N:12]3[CH2:13][CH2:14][CH:9]([C:6]4[C:5]5[CH:27]=[CH:28][C:2]([F:1])=[CH:3][C:4]=5[O:8][N:7]=4)[CH2:10][CH2:11]3)=[C:18]([CH3:26])[S:19][C:20]=2[CH2:21]1)(=[O:36])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 7412Benzoyl chlorideHCID 214719903-(2-(4-(6-Fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine

생성물 1

HCID 214719626-Benzoyl-3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine수율 63.5%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 8471Triethylamine용매

실험 절차

To a mixture of 0.5 g of 3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine in 0.5 ml of triethylamine and 10 ml of chloroform was added 0.18 g of benzoyl chloride under cooling and the mixture was stirred for an hour, and then poured into water. The organic layer was washed with water, dried and concentrated. The residue was purified by column chromatography to give 0.4 g of 6-benzoyl-3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine as an oil, m.p. 192°-195° C. as oxalate 1/4 hydrate thereof.

후처리

  1. temperatureunder cooling
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-aef0e4c3bbf34e35aa17f77d38402746
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532240

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