Acetone → HCID 20382884、化合物

HRID 2163231ノート

反応式

HRID 2163231 の反応式
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:17]=[CH:16][C:9]([C:10]([NH:12][CH2:13][CH2:14][OH:15])=[O:11])=[CH:8][CH:7]=1)=[O:4].[S:18]1C=CC=C1CC([O-])=O.[K+].[CH3:28][C:29](C)=[O:30]>>[C:29]([S:18][CH2:2][C:3]([NH:5][C:6]1[CH:17]=[CH:16][C:9]([C:10]([NH:12][CH2:13][CH2:14][OH:15])=[O:11])=[CH:8][CH:7]=1)=[O:4])(=[O:30])[CH3:28]

参加物

4

反応物 3

HCID 180AcetoneHCID 203829064-(2-Chloroacetamido)-N-(2-hydroxyethyl)benzamideHCID 23696799Potassium 2-thienylacetate

生成物 1

HCID 20382884HCID 20382884、化合物収率 57%

実験手順

Compound 8 -- A mixture of 4-(2-chloroacetamido)-N-(2-hydroxyethyl)benzamide (39.3 g., 0.153 mole) and potassium thiolacetate (18.3 g., 0.16 mole) in 650 ml. of acetone is heated at reflux temperature for a period of 2 hr. After standing overnight, the reaction mixture is filtered, the filtercake washed with acetone, slurried with water, filtered and the filtercake washed with water and dried to afford 34.7 g. of crude product. Crystallization of this material from ethyl acetate-methanol affords analytically pure 4-[2-(ACETYLTHIO)ACETAMIDO]-N-(2-HYDROXYETHYL)BENZAMIDE, m.p. 190.0°-192.0° C. (corr.) in 57% yield.

後処理

  1. temperatureat reflux temperature for a period of 2 hr
  2. filtrationthe reaction mixture is filtered
  3. washthe filtercake washed with acetone
  4. filtrationfiltered
  5. washthe filtercake washed with water
  6. customdried
  7. customto afford 34.7 g
  8. customCrystallization of this material from ethyl acetate-methanol

出典と根拠

ORDレコード
ord-b6e4216c03f04c48be804aa4c3b9338b
出典データセット
uspto-grants-1979_01
特許番号
US04132802

反応ノート

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