Potassium Carbonate → HCID 86668652, 화합물

HRID 73611노트

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HRID 73611 반응식
[CH2:1]([N:8]([CH2:16][C:17]#[N:18])[C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C:10]1=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Li].[CH2:20]([O:22][CH:23]=[CH2:24])[CH3:21].C(=O)([O-])[O-].[K+].[K+]>C1COCC1>[CH2:1]([N:8]([CH2:16][C:17]#[N:18])[C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C@@:10]1([C:20]([O:22][CH2:23][CH3:24])=[CH2:21])[OH:15])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 86668650HCID 86668650, 화합물HCID 86668653HCID 86668653, 화합물

생성물 1

HCID 86668652HCID 86668652, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

To {benzyl[(1R)-2-oxocyclohexyl]amino}acetonitrile (298 mg, 1.230 mmol) in THF (9 ml) at −78° C. was added ethylvinyl ether lithium (7.38 ml, 3.69 mmol) in THF via a cannula dropwise over 25 min. The reaction mixture was stirred for an addition 40 min at −78° C. before wet THF (THF/Water 10/1, 10 ml) was added. The reaction was allowed to warm to room temperature. The mixture was cooled, aqueous potassium carbonate (saturated, 10 mL) was added and the mixture was extracted with ethyl acetate (3×20 mL). The combined organic fractions were washed with brine (saturated, 30 mL), dried, filtered and the solvent was evaporated under reduced pressure to give the title compound. The crude product was used directly without further purification in the next step.

후처리

  1. additionwas added
  2. temperatureThe mixture was cooled
  3. extractionthe mixture was extracted with ethyl acetate (3×20 mL)
  4. washThe combined organic fractions were washed with brine (saturated, 30 mL)
  5. customdried
  6. filtrationfiltered
  7. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-94ecfcfedb2a49299be9194fe9b496ee
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829196B2

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