Methyl iodide → HCID 68487035、化合物

HRID 1877997ノート

反応式

HRID 1877997 の反応式
[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

参加物

8

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 477131HCID 477131、化合物

生成物 1

HCID 68487035HCID 68487035、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bf0b4b577389445995679dea38b65816
出典データセット
uspto-grants-2012_11
特許番号
US08314094B2

反応ノート

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