Potassium Carbonate → 1,1-Dimethylethyl N-[(1-ethynylcyclopropyl)sulfonyl]carbamate

HRID 420061

반응식

HRID 420061 반응식
[C:1]([NH:8][S:9]([C:12]1([CH:15]=O)[CH2:14][CH2:13]1)(=[O:11])=[O:10])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[C:17]([O-])([O-])=O.[K+].[K+].C/C(/[O-])=C(/P(OC)(OC)=O)\[N+]#N>CO>[C:1]([NH:8][S:9]([C:12]1([C:15]#[CH:17])[CH2:14][CH2:13]1)(=[O:11])=[O:10])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 578166791108658-38-3HCID 178502985HCID 178502985, 화합물

생성물 1

HCID 578166891,1-Dimethylethyl N-[(1-ethynylcyclopropyl)sulfonyl]carbamate수율 85%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a stirred solution of compound 80 (230 mg, 0.92 mmol) in MeOH (5 mL) at 0° C. was added K2CO3 (255 mg, 1.84 mmol), and Ohira-Bestmann reagent (215 g, 1.10 mmol) (Tetr. Lett. 2008, 49, 4454). The mixture was stirred at room temperature for 16 hrs and was concentrated under reduced pressure. Water, EtOAc, and citric acid were added to bring pH to 4-5. Organics were dried over Na2SO4, filtered, and concentrated under reduced pressure to yield compound 81 in 85% yield.

후처리

  1. concentrationwas concentrated under reduced pressure
  2. additionWater, EtOAc, and citric acid were added
  3. dry with materialOrganics were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-50656435da35495c8fb7a297723df239
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093379B2

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