Acetic Acid → HCID 68543913、化合物

HRID 2242916ノート

反応式

HRID 2242916 の反応式
[C:1]([NH:3][CH3:4])#[CH:2].[Cl:5][C:6]1[C:11]([CH:12]=O)=[C:10]([F:14])[C:9]([CH3:15])=[CH:8][CH:7]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C>C(Cl)Cl>[Cl:5][C:6]1[C:11]([CH2:12][N:3]([C:1]#[CH:2])[CH3:4])=[C:10]([F:14])[C:9]([CH3:15])=[CH:8][CH:7]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 12682786-Chloro-2-fluoro-3-methylbenzaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 22945101HCID 22945101、化合物

生成物 1

HCID 68543913HCID 68543913、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of ethynyl-methylamine (98 uL, 1.16 mmol) and 6-chloro-2-fluoro-3-methyl-benzaldehyde (200 mg, 1.16 mmol) in CH2Cl2 (3 mL) was added sodium triacetoxyborohydride (369 mg, 1.74 mmol) and acetic acid (7 uL, 0.12 mmol). The reaction mixture was stirred at room temperature for 2 hours, quenched with saturated aqueous NaHCO3, and extracted with ethyl acetate. The combined organic phases were washed with brine, dried over anhydrous magnesium sulfate, and concentrated to afford the title compound as yellow oil.

後処理

  1. customquenched with saturated aqueous NaHCO3
  2. extractionextracted with ethyl acetate
  3. washThe combined organic phases were washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-b6d175634c4f44cca56e58963d37d3f5
出典データセット
uspto-grants-2010_03
特許番号
US07674791B2

反応ノート

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