Phenol → 3-(3-Cyanophenyl)-5-(phenoxymethyl)benzoic acid methyl ester

HRID 1699737노트

반응식

HRID 1699737 반응식
[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([CH2:10][OH:11])[CH:7]=[C:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]#[N:19])[CH:13]=2)[CH:5]=1.[C:21]1(O)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(OC(N=NC(OCC)=O)=O)C>C1COCC1>[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([CH2:10][O:11][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:7]=[C:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]#[N:19])[CH:13]=2)[CH:5]=1

참가 물질

6

반응물 4

HCID 996PhenolHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 9881809HCID 9881809, 화합물

생성물 1

HCID 155499623-(3-Cyanophenyl)-5-(phenoxymethyl)benzoic acid methyl ester수율 80.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

30 mg of the 3-(3-cyanophenyl)-5-(hydroxymethyl)benzoic acid methyl ester produced in the production example 4 was dissolved in dry THF in the atmosphere of nitrogen, mixed with 10.5 mg of phenol, 35.4 mg of triphenylphosphine and 21 μl of azodicarboxylic acid diethyl ester at room temperature, and then stirred at room temperature overnight. The solvent was distilled away, and the residue was purified by silica gel chromatography to obtain 31 mg (77%) of the title compound (colorless, crystal).

후처리

  1. distillationThe solvent was distilled away
  2. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-3a218d2e5b0942f0a8ebff439558be5b
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06348478B1

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