Isopropyl iodide → HCID 53978012, 화합물

HRID 442679노트

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HRID 442679 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:14]3[CH:15]=[C:16]4[O:21][CH2:20][O:19][C:17]4=[CH:18][C:13]=3[CH2:12][C:11](=[O:22])[NH:10][N:9]=2)=[CH:4][CH:3]=1.I[CH:24]([CH3:26])[CH3:25]>CN(C=O)C.CCOC(C)=O>[CH:24]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:14]3[CH:15]=[C:16]4[O:21][CH2:20][O:19][C:17]4=[CH:18][C:13]=3[CH2:12][C:11](=[O:22])[NH:10][N:9]=2)=[CH:4][CH:3]=1)([CH3:26])[CH3:25]

참가 물질

5

반응물 2

HCID 6362Isopropyl iodideHCID 9839097HCID 9839097, 화합물

생성물 1

HCID 53978012HCID 53978012, 화합물수율 48.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
65 °C

실험 절차

To a solution of 1-(4-aminophenyl)-7,8-methylenedioxy-3,5-dihydro-2,3-benzodiazepin-4(4H)-one (110 mg, 0.373 mmol) in DMF (3 mL) was added 2-iodopropane (290 μL, 2.91 mmol). The mixture was stirred at 65° C. for two days, diluted with EtOAc (45 mL), washed with water and brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by chromatography to afford the title compound as a tan solid (60 mg, 0.18 mmol, 48%), mp: 144°-146° C. 1H NMR (CDCl3) 8.20 (s, 1H), 7.41 (d, J=8.5, 2H), 6.81 (s, 1H), 6.74 (s, 1H), 6.56 (d, J=8.5, 2H), 6.02 (s, 2H), 3.80 (s, 1H), 3.69 (m, 1H), 3.42 (s, 2H), 1.24 (d, J=6.0, 6H).

후처리

  1. washwashed with water and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by chromatography

출처 및 근거

ORD 기록
ord-a956b3b8b16c4cfaa2b2181483597404
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05891871

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