Triethyl phosphite → HCID 20199967, compound

HRID 979394Notes

Reaction equation

HRID 979394 reaction equation
[CH3:1][C:2]1([CH3:15])[CH2:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([O:11][CH2:12][CH2:13]Cl)[C:4]=2[O:3]1.[CH2:16]([O:18][P:19]([O:23]CC)[O:20][CH2:21][CH3:22])[CH3:17]>>[CH2:16]([O:18][P:19]([CH2:13][CH2:12][O:11][C:10]1[C:4]2[O:3][C:2]([CH3:15])([CH3:1])[CH2:6][C:5]=2[CH:7]=[CH:8][CH:9]=1)(=[O:23])[O:20][CH2:21][CH3:22])[CH3:17]

Participants

3

Reactant 2

HCID 31215Triethyl phosphiteHCID 16109514HCID 16109514, compound

Product 1

HCID 20199967HCID 20199967, compound

Procedure

68.2 g. (0.3 mole) 2,3-dihydro-2,2-dimethyl-7-(2'-chloro-ethoxy)-benzofuran (prepared according to Examples 1 or 2) and 49.86 g. (0.3 mole) triethylphosphite are stirred at 140°-146° C. for 60 hours and heated. When the reaction is completed the obtained yellowish brown oily product is purified by vacuum distillation by distilling off the volatile contaminations at 0.5 torr. The cuts are collected until 148° C. and the distillation residue is a pure product according to gas chromatographic analysis. The product is a pale yellow oily liquid, nD24.5 =1.5101 (compound No. 1).

Workup

  1. temperatureheated
  2. distillationis purified by vacuum distillation
  3. distillationby distilling off the volatile contaminations at 0.5 torr
  4. customThe cuts are collected until 148° C.

Sources & evidence

ORD record
ord-c7e6133cf10c4ec390cb387c2bb36919
Source dataset
uspto-grants-1987_05
Patent number
US04668274

Reaction notes

Loading…