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

HRID 365961

反応式

HRID 365961 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-3051db69995040959e004c7e42720296
出典データセット
uspto-grants-2000_10
特許番号
US06127570

関連ノート

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