Diethyl Ether → HCID 19090901, compound

HRID 973594Notes

Reaction equation

HRID 973594 reaction equation
[CH:1]([OH:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:12]([P:16](Cl)Cl)([CH3:15])([CH3:14])[CH3:13].C([O:21]CC)C>>[CH:1]([O:4][P:16]([C:12]([CH3:15])([CH3:14])[CH3:13])[OH:21])([CH3:3])[CH3:2]

Participants

5

Reactant 4

HCID 3283Diethyl Ether2×HCID 3776IsopropanolHCID 8471TriethylamineHCID 117690tert-Butyldichlorophosphine

Product 1

HCID 19090901HCID 19090901, compound

Procedure

The starting material is prepared as follows: A mixture of 24.7 g of isopropanol and 17.2 g of triethylamine in 35 ml of diethylether is added drop by drop to 30 g of t-butyldichlorophosphine in 100 ml diethylether. The temperature is kept between 5° to 10°. The solid is filtered off and the filtrate evaporated. The crude oil is purified by distillation to yield t-butylphosphonous acid-isopropylester as an oil, b.p. 82°/2 kPa, nD20 =1.4222.

Workup

  1. customThe starting material is prepared
  2. customis kept between 5° to 10°
  3. filtrationThe solid is filtered off
  4. customthe filtrate evaporated
  5. distillationThe crude oil is purified by distillation

Sources & evidence

ORD record
ord-14f5ef5751e9452c87bcfb46ef1579f8
Source dataset
uspto-grants-1991_11
Patent number
US05064819

Reaction notes

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