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Dimethylformamide → HCID 20396643、化合物

HRID 972123
ノート
印刷プレビュー

反応式

HRID 972123 の反応式
[SH:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.CN(C)C=O.Cl[CH2:15][CH:16]([O:21][CH2:22][CH2:23][CH3:24])[O:17][CH2:18][CH2:19][CH3:20].[Cl-].[NH4+]>O>[CH2:18]([O:17][CH:16]([O:21][CH2:22][CH2:23][CH3:24])[CH2:15][S:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1)[CH2:19][CH3:20]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 2401474-MercaptophenolHCID 155969831-(2-Chloro-1-propoxyethoxy)propane

生成物 1

HCID 20396643HCID 20396643、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

The S-monosodium salt of 4-mercaptophenol (0.05 mole) and dimethylformamide (75 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and addition funnel. The mixture is stirred until dissolved, and 1-chloro-2,2-dipropoxyethane (0.05 mole) is added dropwise over a period of about 20 minutes. After the addition is completed, the reaction mixture is blanketed with nitrogen gas and is heated at about 90° C. with stirring for a period of about 48 hours. After this time water (200 ml) is added, and the reaction mixture is neutralized with ammonium chloride. The reaction mixture is then extracted with chloroform, and the organic phase is separated from the aqueous phase. The organic phase is then stripped of solvent, leaving an oil. This oil is distilled under reduced pressure to yield the desired product 4-(2,2-dipropoxyethylthio)phenol.

後処理

  1. customequipped with a mechanical stirrer
  2. additionthermometer and addition funnel
  3. dissolutionuntil dissolved
  4. additionAfter the addition
  5. stirringwith stirring for a period of about 48 hours
  6. extractionThe reaction mixture is then extracted with chloroform
  7. customthe organic phase is separated from the aqueous phase
  8. customleaving an oil
  9. distillationThis oil is distilled under reduced pressure

出典と根拠

ORDレコード
ord-de5f463faa95438086c82764a962f193
出典データセット
uspto-grants-1979_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04163112

反応ノート

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