Methylparaben → HCID 14297705, 화합물

HRID 275243노트

반응식

HRID 275243 반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][CH:3]=1.[F:12][C@@H:13]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:14]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>O1CCCC1>[F:12][C@@H:13]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:14][O:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 7456MethylparabenHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 11137325(S)-2-fluorooctane-1-ol

생성물 1

HCID 14297705HCID 14297705, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

0.1 mol of methyl 4-hydroxybenzoate, 0.1 mol of (S)-2-fluoro-1-octanol and 0.12 mol of triphenylphosphine are dissolved in 250 ml of tetrahydrofuran, and 0.12 mol of diethyl azodicarboxylate is added dropwise with stirring and ice cooling. The mixture is allowed to warm to room temperature, and is then stirred for a further 8 hours. The solvent is then distilled, and the methyl 4-(2-fluorooctyloxy)benzoate is purified by column chromatography. Saponification using aqueous/alcoholic potassium hydroxide solution gives (S)-4-(2-fluorooctyloxy)benzoic acid.

후처리

  1. stirringis then stirred for a further 8 hours
  2. distillationThe solvent is then distilled
  3. customthe methyl 4-(2-fluorooctyloxy)benzoate is purified by column chromatography

출처 및 근거

ORD 기록
ord-51a6dcce5cb84285a9623095259a50f0
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393459

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