Dioxidophosphane → Ethyl p-Anisylphosphonochloridite

HRID 543355노트

반응식

HRID 543355 반응식
P(Cl)[Cl:2].P([O-])[O-].[CH2:7]([P:16](OCC)[O:17][CH2:18][CH3:19])[C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1.C(P(Cl)Cl)C1C=CC(OC)=CC=1>CCOCC>[CH2:7]([P:16]([Cl:2])[O:17][CH2:18][CH3:19])[C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1

참가 물질

6

반응물 4

HCID 12049464DioxidophosphaneHCID 13128761Phosphonous dichlorideHCID 15819877Diethyl p-anisylphosphoniteHCID 57305237p-Anisylphosphonous dichloride

생성물 1

HCID 86740664Ethyl p-Anisylphosphonochloridite

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

This and other phosphonochloridous esters were best prepared by the procedure of Steininger (Chem. Ber., 1962, 95, 2993) for the comproportionation of the corresponding phosphonous dichloride and phosphonite. Thus, a solution of diethyl p-anisylphosphonite (7.5 g, 36 mmol) in dry ether (20 mL) was added to a solution of p-anisylphosphonous dichloride (8.2 g, 36 mmol) in ether (75 mL) at 5° C. The solution was warmed to room temperature and stirred two hours, then concentrated and distilled (Kugelrohr) at 105°-110° C. (0.1 mmHg). Yield: 9.4 g (60%); IR (neat) 1595, 1500, 1255, 1095, 1025, 930, 824 cm-1 ; 1H NMR (CDCl3) δ7.9-7.5 (m, 2H), 8.1-7.8 (m, 2H), 4.0 (m, 2H), 3.82, (s, 3H), 1.30 (t, J=7 Hz, 3H); 31P NMR (CDCl3) δ177.2 (ca. 90%).

후처리

  1. concentrationconcentrated
  2. distillationdistilled (Kugelrohr) at 105°-110° C. (0.1 mmHg)

출처 및 근거

ORD 기록
ord-6e5e9466ab754cfbb909b4a62c9c7ad5
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04661615

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