Chlorosulfonyl isocyanate → HCID 18698847, 화합물

HRID 2289683노트

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HRID 2289683 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 18698847HCID 18698847, 화합물수율 41.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-affc43a758644be1830c83964d674abc
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06093744

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