Methanol → HCID 178443526, 화합물

HRID 265401

반응식

HRID 265401 반응식
[C:1]1([N:7]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:10]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[N:9]=[C:8]2[O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]Br)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:33][P:34]([O:38]CC)[O:35][CH2:36][CH3:37].CO.O>C1(C)C=CC=CC=1>[CH2:36]([CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][O:24][C:8]1[N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:10]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:9]=1)[CH3:37].[CH3:33][PH:34](=[O:35])[O-:38]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 85063Diethyl methylphosphoniteHCID 229164121,4,5-Triphenyl-2-(7-bromoheptyloxy)imidazole

생성물 1

HCID 178443526HCID 178443526, 화합물수율 57.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 1,4,5-triphenyl-2-(7-bromoheptyloxy)-imidazole (1.75 g) and diethyl methylphosphonite (2.45 g) in toluene (10 ml) was heated at reflux temperature for 48 hours. Methanol and water were added and the mixture evaporated to an oil. This was chromatographed on silica gel (ethyl acetate/ethanol). The resulting oil slowly crystallised and was triturated with ether/petroleum ether, filtered then recrystallised from ethanol/ether to give ethyl 7-(1,4,5-triphenyl-imidazol-2-yloxy)heptane-methylphosphinate (1.06 g, 57%) as a white solid, m.p. 101°-2° C. Found: C, 72.05; H, 7.26; N, 5.52%; C31H37N2O3P; Requires: C, 72.07; H, 7.22; N, 5.42%.

후처리

  1. temperatureat reflux temperature for 48 hours
  2. customthe mixture evaporated to an oil
  3. customThis was chromatographed on silica gel (ethyl acetate/ethanol)
  4. customThe resulting oil slowly crystallised
  5. customwas triturated with ether/petroleum ether
  6. filtrationfiltered
  7. customthen recrystallised from ethanol/ether

출처 및 근거

ORD 기록
ord-b4e6be7428ea45bfb31e2b127adfab45
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648373

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