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

HRID 365957

反応式

HRID 365957 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

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 preparative HPLC with acetonitrile:water 9:1 as eluent

出典と根拠

ORDレコード
ord-4dc664032bb44c57911b3f9aacc56af6
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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