Nitric Acid → HCID 18662975, 화합물

HRID 1956175노트

반응식

HRID 1956175 반응식
[CH3:1][C:2]1([CH3:19])[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]1[C:11]1[C:12]([S:17][CH3:18])=[N:13][CH:14]=[N:15][CH:16]=1.[N+:20]([O-])([OH:22])=[O:21].C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH3:1][C:2]1([CH3:19])[CH2:10][C:9]2[C:4](=[CH:5][C:6]([N+:20]([O-:22])=[O:21])=[CH:7][CH:8]=2)[CH:3]1[C:11]1[C:12]([S:17][CH3:18])=[N:13][CH:14]=[N:15][CH:16]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 11430Potassium CarbonateHCID 232269825-(2,2-Dimethyl-2,3-dihydro-1H-inden-1-yl)-4-(methylsulfanyl)pyrimidine

생성물 1

HCID 18662975HCID 18662975, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 30 g (0.11 mol) of 5-(2,2-dimethylindan-1-yl)-4-methylthiopyrimidine in 500 mL of dichloromethane was added dropwise 100 mL of 90 percent nitric acid. After 1 hr the reaction mixture was poured onto a large volume of ice. The mixture was slowly neutralized with solid potassium carbonate and was then extracted with ether. The organic phase was recovered, dried over magnesium sulfate, filtered, and concentrated by evaporation under reduced pressure to obtain 36 g of a tan solid. This was recrystallized from 400 mL of ethyl acetate to obtain 12 g of the title compound as a white solid melting at 167°-168° C.

후처리

  1. additionAfter 1 hr the reaction mixture was poured onto a large volume of ice
  2. extractionwas then extracted with ether
  3. customThe organic phase was recovered
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-099f140587bc41a49f2af5275c73cb3e
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05780465

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