Hexamethylphosphoramide → 9-[4,4-Bis(4-fluorophenyl)butyl]-1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

HRID 647943노트

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HRID 647943 반응식
[CH3:1][C:2]1[C:6]2=[C:7]3[C:11](=[CH:12][CH:13]=[C:5]2[S:4][CH:3]=1)[NH:10][C:9]1[CH2:14][CH2:15][NH:16][CH2:17][C:8]3=1.CN(C)P(=O)(N(C)C)N(C)C.[F:29][C:30]1[CH:35]=[CH:34][C:33]([CH:36]([C:41]2[CH:46]=[CH:45][C:44]([F:47])=[CH:43][CH:42]=2)[CH2:37][CH2:38][CH2:39]I)=[CH:32][CH:31]=1>CN(C)C=O>[F:29][C:30]1[CH:31]=[CH:32][C:33]([CH:36]([C:41]2[CH:42]=[CH:43][C:44]([F:47])=[CH:45][CH:46]=2)[CH2:37][CH2:38][CH2:39][N:16]2[CH2:15][CH2:14][C:9]3[NH:10][C:11]4[C:7]([C:8]=3[CH2:17]2)=[C:6]2[C:2]([CH3:1])=[CH:3][S:4][C:5]2=[CH:13][CH:12]=4)=[CH:34][CH:35]=1

참가 물질

5

반응물 3

HCID 12679HexamethylphosphoramideHCID 1039681,1'-(4-Iodobutylidene)bis[4-fluorobenzene]HCID 20484283HCID 20484283, 화합물

생성물 1

HCID 204843019-[4,4-Bis(4-fluorophenyl)butyl]-1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

2.4 g of 1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole are dissolved in 50 ml of dimethylformamide and 10 ml of hexamethylphosphoric acid triamide 4.5 g of 4,4-bis-(4-fluorophenyl)butyl iodide are added and the mixture is warmed to 80° C. under N2 for 5 hours. The solvent is then evaporated off; the residue is taken up in chloroform, the chloroform mixture is washed with water, dried and evaporated, the residue is chromatographed on Al2O3 with chloroform and the product is recrystallised from isopropanol. Melting point: 158° C.

후처리

  1. customThe solvent is then evaporated off
  2. washthe chloroform mixture is washed with water
  3. customdried
  4. customevaporated
  5. customthe residue is chromatographed on Al2O3 with chloroform
  6. customthe product is recrystallised from isopropanol

출처 및 근거

ORD 기록
ord-9796215c75ee4e54a3d5f7f3e8b9bb95
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410536

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