Ammonia → 4-Benzyloxy-5-methoxy-2-(4-methylbenzoyl)benzonitrile

HRID 2381242ノート

反応式

HRID 2381242 の反応式
[CH2:1]([O:8][C:9]1[C:10]([O:25][CH3:26])=[CH:11][C:12](Br)=[C:13]([C:15]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)=[O:16])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cu][C:28]#[N:29].CN1CCCC1=O.N>O.C(OCC)(=O)C>[CH2:1]([O:8][C:9]1[C:10]([O:25][CH3:26])=[CH:11][C:12]([C:28]#[N:29])=[C:13]([C:15](=[O:16])[C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 222AmmoniaHCID 13387N-methyl-2-pyrrolidoneHCID 53629725(5-Benzyloxy-2-bromo-4-methoxyphenyl)p-tolylmethanoneHCID 178418546HCID 178418546、化合物

生成物 1

HCID 583455504-Benzyloxy-5-methoxy-2-(4-methylbenzoyl)benzonitrile収率 112%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
200 °C

実験手順

A mixture of (5-benzyloxy-2-bromo-4-methoxyphenyl)-p-tolylmethanone (reference example 10-1) (1.11 g), copper(I)cyanide (967 mg) and 1-methyl-2-pyrrolidinone (2 mL) was irradiated with microwave to heat at 200° C. for 10 min while stirring. Water, a 28% ammonia in water and ethyl acetate were added. The separated organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was triturated with diethyl ether to give the title compound (1.08 g).

後処理

  1. customwas irradiated with microwave
  2. dry with materialThe separated organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was triturated with diethyl ether

出典と根拠

ORDレコード
ord-8cc61f0707c54dd58ee417a99f8df97d
出典データセット
uspto-grants-2012_09
特許番号
US08258162B2

反応ノート

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