Triethyl phosphite → 6-Diethylphosphono-2,2-dimethyl-2H-chromene

HRID 275016ノート

反応式

HRID 275016 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][C:7]([CH3:13])([CH3:12])[CH:6]=[CH:5]2.[P:14]([O:21]CC)([O:18][CH2:19][CH3:20])[O:15][CH2:16][CH3:17]>[Ni](Cl)Cl>[CH2:16]([O:15][P:14]([C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][C:7]([CH3:13])([CH3:12])[CH:6]=[CH:5]2)([O:18][CH2:19][CH3:20])=[O:21])[CH3:17]

参加物

4

反応物 2

HCID 31215Triethyl phosphiteHCID 117705336-Bromo-2,2-dimethyl-2H-chromene

生成物 1

HCID 156141666-Diethylphosphono-2,2-dimethyl-2H-chromene

試薬・触媒・溶媒 1

HCID 24385Nickel Dichloride触媒

反応条件

温度
180 °C

実験手順

16 g of 6-bromo-2,2-dimethyl-2H-chromene are dissolved in 100 ml of triethyl phosphite. 2 g of nickel chloride are added and the mixture is refluxed at 180° C. for 24 hours in an autoclave. After the remaining triethyl phosphite has been concentrated, the expected product distills at 130°-140° C. under 0.1 mm Hg. 11.5 g are collected.

後処理

  1. concentrationAfter the remaining triethyl phosphite has been concentrated
  2. distillationthe expected product distills at 130°-140° C. under 0.1 mm Hg
  3. custom11.5 g are collected

出典と根拠

ORDレコード
ord-33d77c441d1e4603a6b6341c3fc08971
出典データセット
uspto-grants-1995_02
特許番号
US05391751

反応ノート

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