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

HRID 420061

反応式

HRID 420061 の反応式
[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]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 578166791108658-38-3HCID 178502985HCID 178502985、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-50656435da35495c8fb7a297723df239
出典データセット
uspto-grants-2012_01
特許番号
US08093379B2

関連ノート

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