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Potassium Iodide → HCID 86749602、化合物

HRID 2294848
ノート
印刷プレビュー

反応式

HRID 2294848 の反応式
C([N:4]1[CH2:10][CH2:9][CH2:8][C:7]2[CH:11]=[C:12]([C:14](=[O:19])[CH2:15][CH2:16][CH2:17]Cl)[S:13][C:6]=2[CH2:5]1)(=O)C.Cl.[F:21][C:22]1[CH:36]=[CH:35][C:25]2[C:26]([CH:29]3[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]3)=[N:27][O:28][C:24]=2[CH:23]=1.[C:37](=[O:40])([O-])[O-].[K+].[K+].[I-].[K+].[CH3:45]N(C)C=O>C1(C)C=CC=CC=1>[C:37]([C:11]1[C:7]2[CH2:8][CH2:9][CH2:10][NH:4][CH2:5][C:6]=2[S:13][C:12]=1[C:14](=[O:19])[CH2:15][CH2:16][CH2:17][N:32]1[CH2:31][CH2:30][CH:29]([C:26]2[C:25]3[CH:35]=[CH:36][C:22]([F:21])=[CH:23][C:24]=3[O:28][N:27]=2)[CH2:34][CH2:33]1)(=[O:40])[CH3:45]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 11334359R-56109 hydrochlorideHCID 21471818HCID 21471818、化合物

生成物 1

HCID 86749602HCID 86749602、化合物

試薬・触媒・溶媒 1

HCID 1140
Toluene
溶媒

反応条件

温度
70 °C

実験手順

A mixture of 2.8 g of 7-acetyl-2-(4-chlorobutyryl)-5,6,7,8-tetrahydro-4H-thieno[2,3-c]azepine, 2.6 g of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine hydrochloride, 3.9 g of potassium carbonate and 1.55 g of potassium iodide in 30 ml of dimethylformamide and 30 ml of toluene was stirred at 70° C. for 20 hours and concentrated in vacuo. To the residue were added ethyl acetate and water, and separated. The ethyl acetate layer was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on a silica gel to give 3.0 g of 7-(acetyl-2-(4-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)butyryl)-5,6,7,8-tetrahydro-4H-thieno[2,3-c]azepine as an oil. The oil was treated with hydrochloric acid in isopropyl alcohol and recrystallized from ethanol-ethyl acetate to give 7-acetyl-2-(4-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)butyryl)-5,6,7,8-tetrahydro-4H-thieno[2,3-c]azepin hydrochloride, m.p. 230° C. (decomposition).

後処理

  1. concentrationconcentrated in vacuo
  2. additionTo the residue were added ethyl acetate and water
  3. customseparated
  4. washThe ethyl acetate layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography on a silica gel

出典と根拠

ORDレコード
ord-ae22d9c42005494ca41a050b7c7e83c3
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05691330

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート