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

HRID 1952869

반응식

HRID 1952869 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 232645691-(2,2-Diethoxyethyl)cyclopropane

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 3283Diethyl Ether용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ac349e32008f4c8e8140cd83140d9543
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06114365

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