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Methanol → HCID 57642349, 화합물

HRID 2112488
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HRID 2112488 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([F:20])[C:17](F)=[CH:18][C:13]=2[NH:12][C:11](=[O:21])[CH2:10][N:9]=1.[CH3:22][OH:23].[H-].[Na+]>C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([F:20])[C:17]([O:23][CH3:22])=[CH:18][C:13]=2[NH:12][C:11](=[O:21])[CH2:10][N:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 24758Sodium hydrideHCID 57642332HCID 57642332, 화합물

생성물 1

HCID 57642349HCID 57642349, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

A mixture of 0.10 g (0.00033 mole) of 5-(2-chlorophenyl)-7,8-difluoro-1,3-dihydro-2H-1,4-benzodiazepin-2-one (Imm), 2 mL of methanol and 0.03 g of sodium hydride was heated at 100° C. for 40 minutes using microwave heating in a sealed reaction vessel. The mixture was then cooled. diluted with ethyl acetate and washed successively with water and then brine. The mixture was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give 0.103 g of 5-(2-chlorophenyl)-1,3-dihydro-7-fluoro-8-methoxy-2H-1,4-benzodiazepin-2-one (Ia) as a white solid. MH+/Z=319.

후처리

  1. temperatureusing microwave heating in a sealed reaction vessel
  2. temperatureThe mixture was then cooled
  3. washwashed successively with water
  4. dry with materialThe mixture was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d407f3efcdd04d8e8102cd8f7f27d37c
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07524840B2

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