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Potassium Iodide → HCID 86749602, 화합물

HRID 1734073
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HRID 1734073 반응식
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]
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참가 물질

7

반응물 5

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 11334359R-56109 hydrochlorideHCID 21471818HCID 21471818, 화합물

생성물 1

HCID 86749602HCID 86749602, 화합물

시약·촉매·용매 1

HCID 1140
Toluene
용매

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온도
70 °C

실험 절차

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-l,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]azepine hydrochloride, m.p. 230° C. (decomposition).

후처리

  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

출처 및 근거

ORD 기록
ord-46f324ede31f4ed6a603f7215128eb64
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05532240

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