Thiophosgene → 4-Isopropoxy-3-isothiocyanato-benzenesulfonamide

HRID 333586ノート

反応式

HRID 333586 の反応式
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]

参加物

6

反応物 3

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

生成物 1

HCID 866653704-Isopropoxy-3-isothiocyanato-benzenesulfonamide

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fc165a36b5d44f3492a4ade0d8299700
出典データセット
uspto-grants-2014_11
特許番号
US08883473B2

反応ノート

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