Thiophosgene → 4-Isopropoxy-3-isothiocyanato-benzenesulfonamide

HRID 2403037노트

반응식

HRID 2403037 반응식
C(=O)(O)[O-].[Na+].[NH2:6][C:7]1[CH:8]=[C:9]([S:17]([NH2:20])(=[O:19])=[O:18])[CH:10]=[CH:11][C:12]=1[O:13][CH:14]([CH3:16])[CH3:15].[C:21](Cl)(Cl)=[S:22]>O.C(Cl)(Cl)Cl>[CH:14]([O:13][C:12]1[CH:11]=[CH:10][C:9]([S:17]([NH2:20])(=[O:18])=[O:19])=[CH:8][C:7]=1[N:6]=[C:21]=[S:22])([CH3:16])[CH3:15]

참가 물질

6

반응물 3

HCID 10040ThiophosgeneHCID 516892Sodium BicarbonateHCID 696691073-Amino-4-isopropoxy-benzenesulfonamide

생성물 1

HCID 866653704-Isopropoxy-3-isothiocyanato-benzenesulfonamide

시약·촉매·용매 2

HCID 962Water용매2회HCID 6212Chloroform용매

실험 절차

A solution of sodium bicarbonate (16.8 g, 199.5 mmol) in water (400 mL) was added to 3-amino-4-isopropoxy-benzenesulfonamide (15.3 g, 66.5 mmol, example 2, step d) in a mixture of chloroform (200 mL) and water (200 mL). Thiophosgene (6.37 mL, 83.1 mmol) was then added. The biphasic solution was stirred at room temperature for 1.5 h. The phases were separated and the aqueous phase was extracted with CH2Cl2. The organic phase was washed with water, dried (Na2SO4), filtered, and concentrated, yielding the crude title compound as a tan solid.

후처리

  1. customThe phases were separated
  2. extractionthe aqueous phase was extracted with CH2Cl2
  3. washThe organic phase was washed with water
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4d169644f1684afb898e58993cb9d556
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08798939B2

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