Diethylamine → 2-Chloro-N,N-diethylnicotinamide

HRID 1801493

反応式

HRID 1801493 の反応式
[Cl:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH2:11]([NH:13][CH2:14][CH3:15])[CH3:12]>ClCCl>[Cl:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([N:13]([CH2:14][CH3:15])[CH2:11][CH3:12])=[O:5]

参加物

4

反応物 2

HCID 8021DiethylamineHCID 27745412-Chloronicotinoyl chloride

生成物 1

HCID 44659442-Chloro-N,N-diethylnicotinamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-chloronicotinoyl chloride (20.0 g, 114.3 mmol) in dichloromethane (100 mL) at 0° C. was added diethylamine (23.7 mL, 228.6 mmol). The reaction mixture was stirred overnight at room temperature, washed with water (3×100 mL), dried over sodium sulfate and concentrated under reduced pressure to provide the desired product as a brown oil. LC MS: 213 [M+H]. The crude product was used in Step 2 without any further purification.

後処理

  1. washwashed with water (3×100 mL)
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-7f887e8b1a2647beba2c6d228f3f17eb
出典データセット
uspto-grants-2013_01
特許番号
US08349827B2

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