Formaldehyde → Ethyl 2-methylidenebutanoate

HRID 362440

반응식

HRID 362440 반응식
[CH3:1][CH2:2][CH:3](P(OCC)(OCC)=O)[C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:17]([O-])([O-])=O.[K+].[K+].C=O.O>CCOCC>[CH2:17]=[C:3]([CH2:2][CH3:1])[C:4]([O:6][CH2:7][CH3:8])=[O:5]

참가 물질

6

반응물 4

HCID 712FormaldehydeHCID 962WaterHCID 11430Potassium CarbonateHCID 229053Ethyl 2-(diethoxyphosphoryl)butanoate

생성물 1

HCID 291416Ethyl 2-methylidenebutanoate수율 87%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
80 °C

실험 절차

A mixture of 5.0 g (0.019 mol) of triethyl 2-phosphonobutyrate, 5.5 g (0.039 mol) of K2CO3, 6.2 g (0.076 mol) of 37% aqueous formaldehyde solution, and 15 mL of water was heated to about 80° C. for about 45 min. After cooling to RT, 75 mL of ether was added and the organic layer was separated, washed with brine (1×20 mL), dried (MgSO4), and filtered. The ether was carefully removed by distillation, leaving behind 2.1 g (87%) of the title compound as a clear oil which was used directly without further purification. 1H NMR (CDCl3): 67 1.01 (3H, t, J=7), 1.24 (3H, t, J=7), 2.26 (2H, q, J=7), 4.14 (2H, q, J=7), 5.45 (1H, s), 6.06 (1H, s).

후처리

  1. temperatureAfter cooling to RT
  2. customthe organic layer was separated
  3. washwashed with brine (1×20 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customThe ether was carefully removed by distillation

출처 및 근거

ORD 기록
ord-b86d1ac0d50847d384b8902fb40aaab5
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05869511

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