Methylparaben → HCID 14297705、化合物

HRID 275243ノート

反応式

HRID 275243 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 14297705HCID 14297705、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-51a6dcce5cb84285a9623095259a50f0
出典データセット
uspto-grants-1995_02
特許番号
US05393459

反応ノート

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