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

HRID 2381242노트

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HRID 2381242 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매2회HCID 8857Ethyl Acetate용매

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온도
200 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8cc61f0707c54dd58ee417a99f8df97d
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258162B2

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