Dimethyl Sulfate → HCID 89620702、化合物

HRID 1499997ノート

反応式

HRID 1499997 の反応式
[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]

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 89620381HCID 89620381、化合物

生成物 1

HCID 89620702HCID 89620702、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6c28bf76b3bf49b2b96d78a20d399b09
出典データセット
uspto-grants-2015_12
特許番号
US09204650B2

反応ノート

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