Hydrochloric Acid → Ethyl valerimidate

HRID 373120

반응식

HRID 373120 반응식
Cl.[C:2](=[NH:10])([O:7][CH2:8][CH3:9])[CH2:3][CH2:4][CH2:5][CH3:6].C(#N)CCCC.C(O)C.Cl>C(=O)([O-])[O-].[K+].[K+]>[C:2](=[NH:10])([O:7][CH2:8][CH3:9])[CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 8061ValeronitrileHCID 12283341Ethyl pentanimidate hydrochloride

생성물 1

HCID 12283340Ethyl valerimidate수율 72%

시약·촉매·용매 1

HCID 11430Potassium Carbonate용매

실험 절차

A 12.7 g (76.7 mmol) sample of ethyl valerimidate hydrochloride (prepared from valeronitrile, ethanol, and hydrogen chloride gas as described by A. J. Hill and I. Rabinowitz, J. Am. Chem. Soc., 1926, 48, 734) was dissolved in 33% (w/w) potassium carbonate solution (made by dissolving 15 g of K2CO3 in 30 mL of H2O) and immediately extracted with either (3×40 mL). The combined ether layers were dried over Na2SO4, filtered, and concentrated in vacuo to give 7.09 g (72%) of the product as a clear oil, which was used directly in the next step. 1H NMR (300 MHz, CDCl3, ppm): δ0.88 (t, J=7 Hz, 3H), 1.24 (t, J=7 Hz, 3H), 1.31 (m, 2H), 1.50 (m, 2H), 2.19 (t, J=7.5 Hz, 2H), 4.06 (q, J=7 Hz, 2H), 6.84 (br s, 1H).

후처리

  1. extractionimmediately extracted with either (3×40 mL)
  2. dry with materialThe combined ether layers were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-97a9658136cb45f4bb2f7ee4fa0bccd3
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05162325

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