Hydroxyphenylacetic acid → HCID 12531839、化合物

HRID 1704028ノート

反応式

HRID 1704028 の反応式
O[C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.ClC1C=CC([CH2:19][S:20]([CH2:23][C:24]2[CH:29]=CC(Cl)=CC=2)(=[O:22])=[O:21])=CC=1.[C:31](=O)([O-])[O-].[K+].[K+].CN(C)[C:39](=[O:41])[CH3:40]>O>[CH3:19][S:20]([C:23]1[CH:24]=[CH:29][C:39]([O:41][C:2]2[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=2)=[CH:40][CH:31]=1)(=[O:21])=[O:22]

参加物

6

反応物 4

HCID 127Hydroxyphenylacetic acidHCID 11430Potassium CarbonateHCID 31374DimethylacetamideHCID 346670Bis[4-chlorobenzyl]sulfone

生成物 1

HCID 12531839HCID 12531839、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 30.4 g of p-hydroxyphenylacetic acid, 38.12 g of p-chlorophenyl methylsulfone, 55.2 g of potassium carbonate and 250 ml of N,N-dimethylacetamide is heated under Argon overnight at 150°-155° C with vigorous stirring. The mixture is cooled, diluted with 500 ml of H2O, and extracted with two 200 ml portions of benzene. Acidification of the aqueous layer affords an amber oil which solidifies to a white solid, mp 122.5°-125° C. Recrystallization from chloroform affords the product as white needles, mp 127.5°-129.5° C.

後処理

  1. temperatureis heated under Argon overnight at 150°-155° C with vigorous stirring
  2. temperatureThe mixture is cooled
  3. extractionextracted with two 200 ml portions of benzene
  4. customAcidification of the aqueous layer affords an amber oil which
  5. customRecrystallization from chloroform

出典と根拠

ORDレコード
ord-1995e95558cc424391aac779e8cb375c
出典データセット
uspto-grants-1978_11
特許番号
US04125729

反応ノート

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