Dimethyl Sulfate → HCID 89620702, 화합물

HRID 1499997노트

반응식

HRID 1499997 반응식
[CH3:1][C:2]1[C:16]([S:17]([CH3:20])(=[O:19])=[O:18])=[C:15]([C:21]([F:24])([F:23])[F:22])[CH:14]=[CH:13][C:3]=1[C:4]([NH:6][C:7]1[O:8][C:9]([CH3:12])=[N:10][N:11]=1)=[O:5].[C:25]([O-])([O-])=O.[K+].[K+].S(OC)(OC)(=O)=O>CN(C=O)C>[CH3:25][N:6]([C:7]1[O:8][C:9]([CH3:12])=[N:10][N:11]=1)[C:4](=[O:5])[C:3]1[CH:13]=[CH:14][C:15]([C:21]([F:24])([F:23])[F:22])=[C:16]([S:17]([CH3:20])(=[O:19])=[O:18])[C:2]=1[CH3:1]

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 89620381HCID 89620381, 화합물

생성물 1

HCID 89620702HCID 89620702, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

180 mg (0.495 mmol) of 2-methyl-N-(5-methyl-1,3,4-oxadiazol-2-yl)-3-(methylsulfonyl)-4-(trifluoromethyl)benzamide are dissolved in 6 ml of DMF (abs.), and 68 mg (0.495 mmol) of K2CO3 and 0.047 ml (0.495 mmol) of dimethyl sulfate are added. The reaction mixture is boiled under reflux for 15 hours. Then the mixture is filtered, and the filtrate is concentrated and purified by column chromatography (silica gel; heptane/ethyl acetate).

후처리

  1. temperatureunder reflux for 15 hours
  2. filtrationThen the mixture is filtered
  3. concentrationthe filtrate is concentrated
  4. custompurified by column chromatography (silica gel; heptane/ethyl acetate)

출처 및 근거

ORD 기록
ord-6c28bf76b3bf49b2b96d78a20d399b09
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09204650B2

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