Phosphorus oxide (P4O10) → 5-Bromo-6,6'-dimethyl-2-pivaloyloxy-2',3',4'-trimethoxybenzophenone

HRID 365961

반응식

HRID 365961 반응식
[C:1]([O:7][C:8]1[CH:16]=[CH:15][C:14]([Br:17])=[C:13]([CH3:18])[C:9]=1[C:10]([OH:12])=O)(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].[CH3:19][O:20][C:21]1[CH:22]=[C:23]([CH3:31])[CH:24]=[C:25]([O:29][CH3:30])[C:26]=1[O:27][CH3:28].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>ClCCl>[Br:17][C:14]1[CH:15]=[CH:16][C:8]([O:7][C:1](=[O:6])[C:2]([CH3:3])([CH3:4])[CH3:5])=[C:9]([C:13]=1[CH3:18])[C:10]([C:22]1[C:23]([CH3:31])=[CH:24][C:25]([O:29][CH3:30])=[C:26]([O:27][CH3:28])[C:21]=1[O:20][CH3:19])=[O:12]

참가 물질

5

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 809223,4,5-TrimethoxytolueneHCID 232932342-Pivaloyloxy-5-bromo-6-methylbenzoic acid

생성물 1

HCID 226713735-Bromo-6,6'-dimethyl-2-pivaloyloxy-2',3',4'-trimethoxybenzophenone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 50A (6.3 g, 20 mmol), 3,4,5-trimethoxytoluene (3.83 g; 21 mmol), P2O5 (12.0 g) and dichloromethane (100 ml) is stirred at room temperature for 16 hours. Subsequently, the dichloromethane is distilled off and the residue is diluted with water and ethyl acetate. The organic phase is washed with water and concentrated. The residue is purified by flash chromatography with petrol ethers/ethyl acetate (9:1 v/v) as eluent yielding the pure product as white crystals, 5.58 g, (58.2%).

후처리

  1. distillationSubsequently, the dichloromethane is distilled off
  2. additionthe residue is diluted with water and ethyl acetate
  3. washThe organic phase is washed with water
  4. concentrationconcentrated
  5. customThe residue is purified by flash chromatography with petrol ethers/ethyl acetate (9:1 v/v) as eluent

출처 및 근거

ORD 기록
ord-3051db69995040959e004c7e42720296
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127570

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