N-Methylcyclohexylamine → 4-Chloro-N-cyclohexyl-N-methylbutanamide

HRID 35247

반응식

HRID 35247 반응식
C(OCC)(=O)C.[CH3:7][NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.[Cl:15][CH2:16][CH2:17][CH2:18][C:19](Cl)=[O:20].C(N(CC)CC)C>O>[CH3:7][N:8]([CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)[C:19](=[O:20])[CH2:18][CH2:17][CH2:16][Cl:15]

참가 물질

6

반응물 4

HCID 7514N-MethylcyclohexylamineHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 783704-Chlorobutyryl chloride

생성물 1

HCID 132082974-Chloro-N-cyclohexyl-N-methylbutanamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To ethyl acetate (400 ml) is added N-methylcyclohexylamine (26 ml), and to the mixture are added dropwise with stirring 4-chlorobutyryl chloride (25 ml) and triethylamine (33.5 ml) over a period of 20 minutes with keeping the inner temperature at 10° to 20° C. by ice-cooling. The mixture is further stirred at room temperature for one hour. After the reaction, water is added to the reaction mixture. The organic layer is separated and washed with water an aqueious saturated potassium carbonate solution, 10% aqueous hydrochloric acid and water in order, and then dried over anhydrous sodium sulfate. After filtering off sodium sulfate, the mother liquor is concentrated and distilled under reduced pressure to give N-methyl-N-cyclohexyl-4-chlorobutyramide (41.5 g), b.p. 133°-136° C./2 mmHg.

후처리

  1. customat 10° to 20° C.
  2. temperaturecooling
  3. additionis added to the reaction mixture
  4. customThe organic layer is separated
  5. washwashed with water an aqueious saturated potassium carbonate solution, 10% aqueous hydrochloric acid and water in order
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationAfter filtering off sodium sulfate
  8. concentrationthe mother liquor is concentrated
  9. distillationdistilled under reduced pressure

출처 및 근거

ORD 기록
ord-d3926ad918984844bf5b7332cf93bba8
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766120

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