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 2294816ノート

反応式

HRID 2294816 の反応式
[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

参加物

6

反応物 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

生成物 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]pyridine収率 63.5%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8471Triethylamine溶媒

実験手順

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 chlomatogaphy 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 1/4hydrate thereof.

後処理

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

出典と根拠

ORDレコード
ord-87475abca1ed4cf3847e37936cbeb5b4
出典データセット
uspto-grants-1997_11
特許番号
US05691330

反応ノート

読み込み中…