Methyl iodide → HCID 68487035, 화합물

HRID 1877997노트

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HRID 1877997 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:10][C:9](=[O:11])[O:8][C:7]([C:14]([F:17])([F:16])[F:15])([CH:12]=[CH2:13])[C:6]=2[CH:18]=1.[H-].[Na+].[CH3:21]I.[Cl-].[NH4+]>CN(C=O)C.C(OCC)(=O)C.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:10]([CH3:21])[C:9](=[O:11])[O:8][C:7]([C:14]([F:15])([F:16])[F:17])([CH:12]=[CH2:13])[C:6]=2[CH:18]=1

참가 물질

8

반응물 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 477131HCID 477131, 화합물

생성물 1

HCID 68487035HCID 68487035, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a stirred solution of 6-chloro-4-(trifluoromethyl)-4-vinyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (100 mg, 0.36 mmol) in DMF (1 mL), sodium hydride (60%, 29 mg, 0.72 mmol) were added at 0° C. After the mixture was stirred at 0° C. for 30 minutes, methyl iodide (44.8 μL, 0.72 mmol) was added dropwise thereto. After the reaction solution was stirred overnight at room temperature, water was added thereto. The solution was diluted with ethyl acetate and a saturated aqueous ammonium chloride solution was added thereto. The organic layer was separated and washed with saturated brine and then dried over magnesium sulfate. After the drying agent was removed by filtration, the solvent was evaporated under reduced pressure, whereby the objective compound (107 mg, quant.) was obtained as a pale brown solid.

후처리

  1. stirringAfter the reaction solution was stirred overnight at room temperature
  2. customThe organic layer was separated
  3. washwashed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. customAfter the drying agent was removed by filtration
  6. customthe solvent was evaporated under reduced pressure, whereby the objective compound (107 mg, quant.)
  7. customwas obtained as a pale brown solid

출처 및 근거

ORD 기록
ord-bf0b4b577389445995679dea38b65816
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314094B2

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