Chloroiodomethane → Di-tert-butyl (chloromethyl) phosphate

HRID 20210

反応式

HRID 20210 の反応式
[P:1]([O-:13])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[Cl:14][CH2:15]I>C1C=CC=CC=1>[P:1]([O:13][CH2:15][Cl:14])([O:3][C:4]([CH3:6])([CH3:7])[CH3:5])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:2]

参加物

4

反応物 2

HCID 11644ChloroiodomethaneHCID 4191557Ditert-butyl phosphate

生成物 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

The tetrabutylammonium salt of bis-tert butyl phosphate (45.1 g, 0.1 mol) and chloroiodomethane (200 g, 1.14 mol) were combined in 100 ml of benzene and the mixture was stirred at room temperature for four hours and then the benzene was removed under vacuum. A portion of 500 ml of ethyl ether was added to the residue and insoluble solid was filtered away. Concentration of the filtrate in vacuo and removal of the volitiles on a vacuum pump provided di-tert-butyl chloromethyl phosphate, as a light yellow or light brown oil which was utilized in the next step without further purification.

後処理

  1. customthe benzene was removed under vacuum
  2. additionA portion of 500 ml of ethyl ether was added to the residue and insoluble solid
  3. filtrationwas filtered away
  4. customConcentration of the filtrate in vacuo and removal of the volitiles on a vacuum pump

出典と根拠

ORDレコード
ord-13f9a7cc73b54c34b671626294596dc9
出典データセット
uspto-grants-2010_06
特許番号
US07745625B2

関連ノート

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