Hydrochloric Acid → HCID 11301002、化合物

HRID 1080914ノート

反応式

HRID 1080914 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:6]=1[OH:15])([CH3:4])([CH3:3])[CH3:2].[C:16]([OH:20])(=[O:19])[CH:17]=O.[ClH:21]>C(O)(=O)C.C(O)C>[C:11]([C:7]1[CH:8]=[C:9]([CH:17]([Cl:21])[C:16]([OH:20])=[O:19])[CH:10]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[C:6]=1[OH:15])([CH3:14])([CH3:13])[CH3:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 760Glyoxylic AcidHCID 314052,6-Di-tert-butylphenol

生成物 1

HCID 11301002HCID 11301002、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

反応条件

温度
180 °C

実験手順

65 g of still wet (3,5-di-tert-butyl-4-hydroxy-phenyl)-chloroacetic acid are prepared from 41.2 g (0.2 mol) of 2,6-di-tert-butylphenol, 35.4 g (0.24 mol) of 50% aqueous glyoxylic acid and 44 g of hydrogen chloride in 200 ml of acetic acid as described in Example 2A. This acid is dissolved in 200 ml of absolute ethanol and allowed to stand overnight. The solvent is then evaporated in vacuo, 1.0 g of p-toluenesulfonic acid is added, followed by another 200 ml of absolute ethanol. The mixture is then heated for three hours, and the ethanol is then evaporated. The residue is then stirred at 0.1 mm Hg vacuum with the bath temperature slowly increasing up to 180° C. The title compound distills at a temperature between about 140°-160° C. as a viscous orange liquid in a yield of 27 g.

後処理

  1. customThe solvent is then evaporated in vacuo, 1.0 g of p-toluenesulfonic acid
  2. additionis added
  3. temperatureThe mixture is then heated for three hours
  4. customthe ethanol is then evaporated
  5. distillationThe title compound distills at a temperature between about 140°-160° C. as a viscous orange liquid in a yield of 27 g

出典と根拠

ORDレコード
ord-653dc58a08b0489b8dd5e7e12dc2af9a
出典データセット
uspto-grants-1996_12
特許番号
US05583247

反応ノート

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