Water → 1-(4-Hydroxyphenylthio)-n-octadecane

HRID 1608546

反応式

HRID 1608546 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:15](Cl)[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].O>CN(C)C=O>[OH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH3:15])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 188151-ChlorooctadecaneHCID 2401474-Mercaptophenol

生成物 1

HCID 221790531-(4-Hydroxyphenylthio)-n-octadecane収率 70%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

Under a nitrogen atmosphere, p-hydroxythiophenol (126 g) was dissolved in N,N-dimethylformamide (600 ml) and thereto was added potassium carbonate (152 g). Thereto was added octadecyl chloride (318 g), followed by heating at 80° C. for 2 hours. After completion of the reaction, the reaction mixture was poured into water to precipitate a white solid. Thereto was added 5% hydrochloric acid to adjust the pH to acidic state and then, the white solid was filtered off under reduced pressure and then recrystallized from methyl ethyl ketone to obtain the desired product (261 g). Yield 70%; m.p. 95° C.

後処理

  1. customAfter completion of the reaction
  2. customto precipitate a white solid
  3. additionThereto was added 5% hydrochloric acid
  4. filtrationthe white solid was filtered off under reduced pressure
  5. customrecrystallized from methyl ethyl ketone

出典と根拠

ORDレコード
ord-ba7ec9f547ea4cb48b338cd02e1cfa2b
出典データセット
uspto-grants-1995_03
特許番号
US05395815

関連ノート

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