反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](O)=[O:7])=[C:4]([Cl:11])[CH:3]=1.CCN(C(C)C)C(C)C.CN([C:24]([O:28][N:29]1N=NC2C=CC=N[C:30]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([N:29]([O:28][CH3:24])[CH3:30])=[O:7])=[C:4]([Cl:11])[CH:3]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a stirring solution of 4-bromo-2-chlorobenzoic acid (3.45 g, 15 mmol) and DIEA (7.7 ml, 44 mmol) in DMF (30 mL) was added HATU (6.1 g, 16 mmol) at 23° C. under nitrogen. Darkened suspension stirred for 1 h, then added n,o-dimethylhydroxylamine hydrochloride (2.1 g, 22 mmol). Solution stirred overnight at 23° C. Reaction then partitioned between 2.5% NaHCO3 (250 mL) and diethyl ether (100 mL). Aqueous further extracted with ether (2×50 mL). Combined ethereal extracts dried over MgSO4, then concentrated an amber oil under reduced pressure. 4-bromo-2-chloro-N-methoxy-N-methylbenzamide isolated as a light amber oil.
後処理
- stirringSolution stirred overnight at 23° C
- customReaction
- customthen partitioned between 2.5% NaHCO3 (250 mL) and diethyl ether (100 mL)
- extractionAqueous further extracted with ether (2×50 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated an amber oil under reduced pressure
出典と根拠
- ORDレコード
- ord-d5ed4a33c06849c1a8e5bfa29170ba08
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524900B2
関連ノート
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