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

HRID 486052

反応式

HRID 486052 の反応式
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

参加物

4

反応物 2

HCID 7965CyclohexylamineHCID 122951-Ethyl hexanedioate

生成物 1

HCID 224484036-(Cyclohexylamino)-6-oxohexanoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8b82665ebe884b4b9d2beb5211d8de2e
出典データセット
uspto-grants-1994_03
特許番号
US05290790

関連ノート

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