Hydrochloric Acid → HCID 19873523、化合物

HRID 465277ノート

反応式

HRID 465277 の反応式
[H-].[Na+].[CH3:3][NH:4][S:5]([N:8]([CH3:11])[O:9][CH3:10])(=[O:7])=[O:6].Cl[S:13]([NH:16][C:17](=[O:25])[O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:15])=[O:14].Cl>CCCCCC.C1COCC1>[CH3:11][N:8]([O:9][CH3:10])[S:5]([N:4]([S:13]([NH:16][C:17](=[O:25])[O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:14])=[O:15])[CH3:3])(=[O:7])=[O:6]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 19873524HCID 19873524、化合物HCID 22058798Phenyl (chlorosulfonyl)carbamate

生成物 1

HCID 19873523HCID 19873523、化合物収率 93.6%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒3 回HCID 8058Hexane溶媒

実験手順

1.15 g (28.8 mmol) of 60% sodium hydride was washed with n-hexane, and dry THF was added, and the mixture was cooled with ice. To this mixture, a THF solution containing 2 g (13 mmol) of N,N'-dimethyl-N'-methoxysulfamide was dropwise added. After stirring the mixture for 10 minutes, a dry THF solution containing 3.21 g (13.6 mmol) of phenyl N-chlorosulfonylcarbamate was dropwise added thereto. The mixture was stirred at room temperature for 7 hours. The reaction mixture was poured into 500 ml of ice water containing 3.5 g of 35% hydrochloric acid and extracted three times with diethyl ether. The diethyl ether layer was washed sequentially with water and a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 4.3 g of phenyl N-[(N-(N-methyl N-methoxyaminosulfonyl)-N-methylamino)sulfonyl]carbamate as slightly yellow oil.

後処理

  1. additionwas added
  2. temperaturethe mixture was cooled with ice
  3. additionwas dropwise added
  4. additionwas dropwise added
  5. stirringThe mixture was stirred at room temperature for 7 hours
  6. extractionextracted three times with diethyl ether
  7. washThe diethyl ether layer was washed sequentially with water
  8. dry with materiala saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate
  9. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-cd1fc3bf358a4e3fb60fdf847c804537
出典データセット
uspto-grants-1992_10
特許番号
US05152824

反応ノート

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