Ammonia → 2-Butyl-1,3-diaza-spiro[4.4]nonan-4-one

HRID 1636978

반응식

HRID 1636978 반응식
N.[NH2:2][C:3]1([C:8]([NH2:10])=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4]1.[CH:11](=O)[CH2:12][CH2:13][CH2:14][CH3:15].CC(CC(C)=O)C>O>[CH2:12]([CH:11]1[NH:10][C:8](=[O:9])[C:3]2([CH2:7][CH2:6][CH2:5][CH2:4]2)[NH:2]1)[CH2:13][CH2:14][CH3:15]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 7909Methyl Isobutyl KetoneHCID 8063PentanalHCID 111160861-Aminocyclopentanecarboxamide

생성물 1

HCID 101980702-Butyl-1,3-diaza-spiro[4.4]nonan-4-one

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

Ammonia solution (20%; 20 g, 0.30 mol.) is added to a solution of 126 g of 1-aminocyclopentanecarboxamide (>98%, 0.98 mol.) in 150 g of water. 86 g of valeraldehyde (0.99 mol.) are then added at 15° C., during which the temperature rises to 32° C. The reaction mixture is heated to 70° C. and stirred for 7 hours at that temperature. 350 ml of MIBK are added to the emulsion, and the mixture is cooled, with stirring, and the organic phase is separated off. The extract is extensively concentrated by evaporation (200 g), and 200 g of n-hexane are added, and the crystals are filtered off. After drying there remain 125 g of 2-butyl-1,3-diaza-spiro [4.4]nonan4-one (HPLC: 98.6%).

후처리

  1. customrises to 32° C
  2. temperaturethe mixture is cooled
  3. stirringwith stirring
  4. customthe organic phase is separated off
  5. concentrationThe extract is extensively concentrated by evaporation (200 g), and 200 g of n-hexane
  6. additionare added
  7. filtrationthe crystals are filtered off
  8. dry with materialAfter drying there remain 125 g of 2-butyl-1,3-diaza-spiro [4.4]nonan4-one (HPLC: 98.6%)

출처 및 근거

ORD 기록
ord-d8e2b96eff55487aafbe579078c77b78
출처 데이터셋
uspto-grants-2000_03
특허 번호
US06037474

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