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

HRID 35247

反応式

HRID 35247 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d3926ad918984844bf5b7332cf93bba8
出典データセット
uspto-grants-1988_08
特許番号
US04766120

関連ノート

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