Dimethylcarbamoyl Chloride → HCID 21444460、化合物

HRID 328232ノート

反応式

HRID 328232 の反応式
[H-].[Na+].O1CCCC1.[CH3:8][C:9]1[CH:10]=[C:11]([OH:23])[CH:12]=[C:13]([CH3:22])[C:14]=1[S:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=1.[CH3:24][N:25]([CH3:29])[C:26](Cl)=[O:27]>O>[CH3:24][N:25]([CH3:29])[C:26](=[O:27])[O:23][C:11]1[CH:12]=[C:13]([CH3:22])[C:14]([S:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=2)=[C:9]([CH3:8])[CH:10]=1

参加物

6

反応物 4

HCID 6598Dimethylcarbamoyl ChlorideHCID 8028Tetrahydrofuran3 回HCID 24758Sodium hydrideHCID 214444563,5-Dimethyl-4-[(pyridin-2-yl)sulfanyl]phenol

生成物 1

HCID 21444460HCID 21444460、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred suspension of 240 mg. of sodium hydride in 20 ml. of dry tetrahydrofuran is added a solution of 2.31 g. of 3,5-dimethyl-4-(2-pyridylthio)phenol in 30 ml. of dry tetrahydrofuran. After the effervescence has subsided, a solution of 1.1 g. of N,N-dimethylcarbamoyl chloride in 10 ml. of dry tetrahydrofuran is added dropwise. The reaction mixture is stirred at ambient temperature for 16 hours, and then under reflux for 4 hours. The reaction mixture is cooled to room temperature, and then diluted with an excess of water. The product is extracted into ethyl acetate. The ethyl acetate is washed with water, dried using anhydrous magnesium sulfate, and then evaporated in vacuo to give crude 3,5-dimethyl-4-(2-pyridylthio)phenyl N,N-dimethylcarbamate. The crude product can be purified further by recrystallization.

後処理

  1. additionTo a stirred suspension of 240 mg
  2. temperatureunder reflux for 4 hours
  3. temperatureThe reaction mixture is cooled to room temperature
  4. extractionThe product is extracted into ethyl acetate
  5. washThe ethyl acetate is washed with water
  6. customdried
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-39913770e708484b8c8abff61f6646fd
出典データセット
uspto-grants-1977_04
特許番号
US04016278

反応ノート

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