Dimethyl Sulfoxide → HCID 13483105、化合物

HRID 2305823ノート

反応式

HRID 2305823 の反応式
C[C:2](C)([O-:4])C.[K+].[N+:7]([CH2:10][CH2:11][CH3:12])([O-])=O.[C:13]([C:15](=[C:20]([CH3:22])[CH3:21])[C:16](OC)=O)#N.CS(C)=[O:25]>>[C:10]([C:11]1([C:12]([O:4][CH3:2])=[O:25])[C:20]([CH3:22])([CH3:21])[C:15]1([CH3:16])[CH3:13])#[N:7]

参加物

5

反応物 4

HCID 679Dimethyl Sulfoxide3 回HCID 79031-NitropropaneHCID 248907Methyl 2-cyano-3-methylcrotonateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 13483105HCID 13483105、化合物

実験手順

The title compound was synthesized similarly to J. Org. Chem. 50 (1985), 2807-2809: 5.6 g (50mmol) of potassium tert-butoxide were initially charged in 15 ml of dimethyl sulfoxide, and 4.4 g (50 mmol) of nitropropane dissolved in 190 ml of dimethyl sulfoxide were slowly added dropwise. After addition of 5 g (36 mmol) of methyl 2-cyano-3-methylbut-2-enoate dissolved in 10 ml of dimethyl sulfoxide, the mixture was stirred at room temperature for 40 hours. The reaction was quenched by slow addition of water. The reaction mixture was extracted three times with methyl tert-butyl ether. The organic phases were dried with magnesium sulfate and freed from ether giving the crude product (9 g), which was employed for the next reaction without any further purification.

後処理

  1. additionwere slowly added dropwise
  2. customThe reaction was quenched by slow addition of water
  3. extractionThe reaction mixture was extracted three times with methyl tert-butyl ether
  4. dry with materialThe organic phases were dried with magnesium sulfate
  5. customwas employed for the next reaction without any further purification

出典と根拠

ORDレコード
ord-d596ae9026f747309866659b016b572f
出典データセット
uspto-grants-2002_08
特許番号
US06441044B1

反応ノート

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