Acetone → N-(3,5-Dichloro-2-hydroxy-4-methylphenyl)acetamide

HRID 2420206

반응식

HRID 2420206 반응식
Cl.[NH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH3:10])=[C:5]([Cl:11])[C:4]=1[OH:12].C(N(CC)C1C=CC=CC=1)C.[CH3:24][C:25](C)=[O:26].C(Cl)(=O)C>O>[C:25]([NH:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH3:10])=[C:5]([Cl:11])[C:4]=1[OH:12])(=[O:26])[CH3:24]

참가 물질

6

반응물 4

HCID 180AcetoneHCID 6367Acetyl chlorideHCID 7061N,N-DiethylanilineHCID 1702236-Amino-2,4-dichloro-m-cresol hydrochloride

생성물 1

HCID 13796880N-(3,5-Dichloro-2-hydroxy-4-methylphenyl)acetamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 68.4 g. of 2-amino-5-methyl-4,6-dichloro-phenol hydrochloride and 96 ml. of N,N-diethylaniline in 750 ml. of acetone, 23.4 ml. of acetyl chloride were added slowly by keeping the temperature under 20° C. At the end, the reaction mixture was heated to reflux for an hour. After cooling, the solution was poured into water; the solid product, thus obtained, was collected on a buckner, washed with water until the washings were neutral and dried in a desicator at 50° C. The raw product obtained was purified by crystallization from ethyl alcohol, yielding 44 g. of a pure product with M.P. = 175°-176.5° C.

후처리

  1. additionTo a mixture of 68.4 g
  2. customunder 20° C
  3. temperatureAt the end, the reaction mixture was heated
  4. temperatureto reflux for an hour
  5. temperatureAfter cooling
  6. customthe solid product, thus obtained
  7. customwas collected on a buckner
  8. washwashed with water until the washings
  9. customdried in a desicator at 50° C

출처 및 근거

ORD 기록
ord-276cb44cd9e64c2f9dbd148d277632b1
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04110116

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