Phosphorus oxide (P4O10) → 2-Acetoxy-5-bromo-6,6'-dimethyl-2', 3', 4'-trimethoxy-benzophenone

HRID 365957

반응식

HRID 365957 반응식
[C:1]([O:4][C:5]1[CH:13]=[CH:12][C:11]([Br:14])=[C:10]([CH3:15])[C:6]=1[C:7]([OH:9])=O)(=[O:3])[CH3:2].[CH3:16][O:17][C:18]1[CH:19]=[C:20]([CH3:28])[CH:21]=[C:22]([O:26][CH3:27])[C:23]=1[O:24][CH3:25].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>ClCCl>[C:1]([O:4][C:5]1[CH:13]=[CH:12][C:11]([Br:14])=[C:10]([CH3:15])[C:6]=1[C:7]([C:19]1[C:20]([CH3:28])=[CH:21][C:22]([O:26][CH3:27])=[C:23]([O:24][CH3:25])[C:18]=1[O:17][CH3:16])=[O:9])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 809223,4,5-TrimethoxytolueneHCID 110111492-Acetoxy-5-bromo-6-methylbenzoic acid

생성물 1

HCID 109062512-Acetoxy-5-bromo-6,6'-dimethyl-2', 3', 4'-trimethoxy-benzophenone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 1C (6.83 g, 25 mmol), 3,4,5-trimethoxytoluene (4.56 g; 25 mmol), P2O5 (15.0 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 preparative HPLC with acetonitrile:water 9:1 as eluent yielding the pure product as a yellow oil, 1.1 g, (10.1%).

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 preparative HPLC with acetonitrile:water 9:1 as eluent

출처 및 근거

ORD 기록
ord-4dc664032bb44c57911b3f9aacc56af6
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127570

연결된 노트

불러오는 중…