Chlorosulfonyl isocyanate → HCID 18698847、化合物

HRID 2289683ノート

反応式

HRID 2289683 の反応式
C(=O)=[N:2][S:3](Cl)(=[O:5])=[O:4].[C:8]([Si:12]([CH3:28])([CH3:27])[O:13][C:14]1[CH:19]=[C:18]([CH:20]([CH3:22])[CH3:21])[C:17]([OH:23])=[C:16]([CH:24]([CH3:26])[CH3:25])[CH:15]=1)([CH3:11])([CH3:10])[CH3:9]>C1(C)C=CC=CC=1>[S:3](=[O:4])(=[O:5])([O:23][C:17]1[C:16]([CH:24]([CH3:26])[CH3:25])=[CH:15][C:14]([O:13][Si:12]([C:8]([CH3:9])([CH3:11])[CH3:10])([CH3:27])[CH3:28])=[CH:19][C:18]=1[CH:20]([CH3:22])[CH3:21])[NH2:2]

参加物

4

反応物 2

HCID 70918Chlorosulfonyl isocyanateHCID 186988374-(Tert-butyl-dimethyl-silanyloxy)-2,6-diisopropylphenol

生成物 1

HCID 18698847HCID 18698847、化合物収率 41.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

N-Chlorosulfonyl isocyanate (3.43 mL, 39.4 mmol) was added to a warm solution of 4-(tert-butyl-dimethyl-silanyloxy)-2,6-diisopropylphenol (11.59 g, 37.6 mmol) in 400 mL toluene. The resulting solution was heated to reflux for 6 hours and then cooled to room temperature and stirred overnight. The reaction was concentrated in vacuo, and the residue was quenched with ice water and extracted with dichloromethane. The organic layer was dried over magnesium sulfate, filtered, and concentrated to give an orange oil. Chromatography on silica gel gave 6.06 g of 4-(tert-butyl-dimethyl-silanyloxy)-2,6-diisopropylphenyl sulfamate as an orange oil.

後処理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 6 hours
  3. concentrationThe reaction was concentrated in vacuo
  4. customthe residue was quenched with ice water
  5. extractionextracted with dichloromethane
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give an orange oil

出典と根拠

ORDレコード
ord-affc43a758644be1830c83964d674abc
出典データセット
uspto-grants-2000_07
特許番号
US06093744

反応ノート

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