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

HRID 1636978

反応式

HRID 1636978 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-d8e2b96eff55487aafbe579078c77b78
出典データセット
uspto-grants-2000_03
特許番号
US06037474

関連ノート

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