Phenyl phosphorus dichloride → O-(2,6-Di-tert-butyl-4-methylphenyl) phenylphosphonochloridite

HRID 224542

반응식

HRID 224542 반응식
[C:1]([C:5]1[C:10]([OH:11])=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:8]=[C:7]([CH3:16])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[Cl:17][P:18](Cl)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(N(CC)CC)C>[C:19]1([P:18]([Cl:17])[O:11][C:10]2[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:6][C:7]([CH3:16])=[CH:8][C:9]=2[C:12]([CH3:15])([CH3:14])[CH3:13])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

4

반응물 2

HCID 12573Phenyl phosphorus dichlorideHCID 314042,6-Di-tert-butyl-4-methylphenol

생성물 1

HCID 53944288O-(2,6-Di-tert-butyl-4-methylphenyl) phenylphosphonochloridite

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To a solution of 110 grams of 2,6-di-tert-butyl-p-cresol in 252 grams of triethylamine was added at 25°-26° C. over a 15-minute period 89.5 grams of dichlorophenylphosphine. The reaction mixture was heated for 31 hours at 95°-97° C. The excess triethylamine solvent was then removed by distillation under vacuum, the resulting residue was triturated with 200 ml of dry benzene, and the white crystalline solid triethylamine hydrochloride was separated by filtration. The desired product named above was isolated from the filtrate by distillation of the benzene under vacuum and crystallization of the residue from acetonitrile. The product was obtained as white crystals melting at 103°-106° C.

후처리

  1. temperatureThe reaction mixture was heated for 31 hours at 95°-97° C
  2. customThe excess triethylamine solvent was then removed by distillation under vacuum
  3. customthe resulting residue was triturated with 200 ml of dry benzene
  4. customthe white crystalline solid triethylamine hydrochloride was separated by filtration
  5. customabove was isolated from the filtrate by distillation of the benzene under vacuum and crystallization of the residue from acetonitrile

출처 및 근거

ORD 기록
ord-303f5b93ae484918862c034fb97dfa07
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04233207

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