Hydroxyphenylacetic acid → HCID 12531839, 화합물

HRID 1704028노트

반응식

HRID 1704028 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 12531839HCID 12531839, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1995e95558cc424391aac779e8cb375c
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04125729

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