Chloroiodomethane → Di-tert-butyl (chloromethyl) phosphate

HRID 20211

反応式

HRID 20211 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>>[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

3

反応物 2

HCID 11644ChloroiodomethaneHCID 4191557Ditert-butyl phosphate

生成物 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate収率 343.6%

実験手順

The tetrabutylammonium salt of bis-tert butyl phosphate (57 g, 0.126 mol, Digital Specialty Chemicals) and chloroiodomethane (221 g, 1.26 mol) were stirred at room temperature for four hours and then the volatiles were removed in vacuo. 500 ml of ethyl ether was added to the residue and insoluble solid was filtered away. Concentration of the filtrate and final removal of volatiles using a vacuum pump provided di-tert-butyl chloromethyl phosphate (112 g), typically as a light yellow or brown oil, which was utilized in the next step without any further purification.

後処理

  1. customthe volatiles were removed in vacuo
  2. addition500 ml of ethyl ether was added to the residue and insoluble solid
  3. filtrationwas filtered away
  4. customConcentration of the filtrate and final removal of volatiles

出典と根拠

ORDレコード
ord-c0ebcf4a032d459780495542121a9694
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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