p-Toluenesulfonic acid → HCID 67172923、化合物

HRID 406963

反応式

HRID 406963 の反応式
[OH:1][CH2:2][C:3]([CH2:8][OH:9])([CH3:7])[C:4]([OH:6])=[O:5].C1(C)C=CC(S(O)(=O)=O)=CC=1.[Cl:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]([C:33]2[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=2)(OC)OC)=[CH:24][CH:23]=1>C1(C)C=CC=CC=1>[Cl:21][C:22]1[CH:23]=[CH:24][C:25]([C:28]2([C:33]3[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=3)[O:9][CH2:8][C:3]([CH3:7])([C:4]([OH:6])=[O:5])[CH2:2][O:1]2)=[CH:26][CH:27]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 78501Dimethylolpropionic acidHCID 11652307Benzene, 1,1'-(dimethoxymethylene)bis[4-chloro-

生成物 1

HCID 67172923HCID 67172923、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

In a round bottom flask, (0.9 g) 3-hydroxy-2-(hydroxymethyl)-2-methylpropanoic acid and (9.8 mg) p-toluene sulfonic acid and 2 ml toluene was taken. The reaction mixture was stirred at room temperature and subsequently 2 g (1 equiv) bis-(4-chlorophenyl)-dimethoxymethane [IIa4] diluted with 5 ml toluene was added through droping funnel. The reaction mixture was heated at reflux temperature and the water was removed azeotropically under Dean Stark. Continuous removal and addition of toluene was done up to 2 hrs. Then the reaction mixture was cooled at room temperature to obtain off white solid. It was filtered and washed with toluene and then water.

後処理

  1. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux temperature
  4. customthe water was removed azeotropically under Dean Stark
  5. customContinuous removal and addition of toluene
  6. temperatureThen the reaction mixture was cooled at room temperature
  7. customto obtain off white solid
  8. filtrationIt was filtered
  9. washwashed with toluene

出典と根拠

ORDレコード
ord-adb7d08ad9a84ddea06d239a776d91c8
出典データセット
uspto-grants-2014_06
特許番号
US08754207B2

関連ノート

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