Thiophosgene → 4-Isopropoxy-3-isothiocyanato-benzenesulfonamide

HRID 405673ノート

反応式

HRID 405673 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-88a9a64b64b14af0895c99db650a07c7
出典データセット
uspto-grants-2014_06
特許番号
US08753857B2

反応ノート

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