Nitrogen → 1-(2,2-Diethoxyethyl)cyclopropane

HRID 1837611

反応式

HRID 1837611 の反応式
[N+](=[CH2:3])=[N-].[CH2:4]([O:6][CH:7]([O:11][CH2:12][CH3:13])[CH2:8][CH:9]=[CH2:10])[CH3:5].N#N>CCOCC.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:4]([O:6][CH:7]([O:11][CH2:12][CH3:13])[CH2:8][CH:9]1[CH2:3][CH2:10]1)[CH3:5]

参加物

6

反応物 3

HCID 947NitrogenHCID 9550DiazomethaneHCID 2564264,4-Diethoxybut-1-ene

生成物 1

HCID 232645691-(2,2-Diethoxyethyl)cyclopropane

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 3283Diethyl Ether溶媒2 回

実験手順

Diazomethane (6.17 g, 147 mmol) was added dropwise to 3.02 g (21 mmol) of 3-butenal diethyl acetal in 10 ml of dry ether with intensive stirring at 0 C. Then 70 mg (0.312 mmol) of palladium (II) acetate in 50 ml of dry ether was added all at once. Then stirring at 0 C continued until the evolution of N2 ceased (10 min.). The ether was distilled off to the reduced volume of the reaction mixture ca 10 ml. The precipitate was filtered off on a fritted glass funnel and the filtrate evaporated. The crude product (2.57 g) contained 97% of the title compound (GC) and was used without further purification.

後処理

  1. stirringThen stirring at 0 C
  2. custom(10 min.)
  3. distillationThe ether was distilled off to the reduced volume of the reaction mixture ca 10 ml
  4. filtrationThe precipitate was filtered off on a fritted glass funnel
  5. customthe filtrate evaporated
  6. customwas used without further purification

出典と根拠

ORDレコード
ord-ffe74f97a18947bf92a7bc54ad5bc33e
出典データセット
uspto-grants-2004_08
特許番号
US06784198B1

関連ノート

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