Cyclohexylamine → 6-(Cyclohexylamino)-6-oxohexanoic acid

HRID 486052

반응식

HRID 486052 반응식
C(O[C:4](=[O:12])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]([OH:11])=[O:10])C.[CH:13]1([NH2:19])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1>O>[CH:13]1([NH:19][C:4](=[O:12])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]([OH:11])=[O:10])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1

참가 물질

4

반응물 2

HCID 7965CyclohexylamineHCID 122951-Ethyl hexanedioate

생성물 1

HCID 224484036-(Cyclohexylamino)-6-oxohexanoic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

34.8 g (0.2 mol) of adipic acid monoethyl ester are added dropwise and with stirring to 19.8 g (0.2 mol) of cyclohexylamine. The temperature rises to 60° C. The reaction mixture is heated to 80° C. for 1 h. After cooling, the solution is poured into 200 ml of water and then extracted with 300 ml of ethyl ether. The ether phase is stirred into 150 ml of potassium hydrogen carbonate solution. After separation of the ether phase when settling has taken place, the aqueous phase is acidified to pH 1 with concentrated hydrochloric acid. The precipitate is drained, washed with water, dried and recrystallised in acetonitrile.

후처리

  1. customrises to 60° C
  2. temperatureAfter cooling
  3. extractionextracted with 300 ml of ethyl ether
  4. customAfter separation of the ether phase when
  5. washwashed with water
  6. customdried
  7. customrecrystallised in acetonitrile

출처 및 근거

ORD 기록
ord-8b82665ebe884b4b9d2beb5211d8de2e
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05290790

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