Ammonia → 4-Isopropoxy-3-thioureidobenzenesulfonamide

HRID 405674ノート

反応式

HRID 405674 の反応式
[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:13])=[O:12])=[CH:7][C:6]=1[N:15]=[C:16]=[S:17])([CH3:3])[CH3:2].[NH3:18]>CO>[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:13])=[O:12])=[CH:7][C:6]=1[NH:15][C:16]([NH2:18])=[S:17])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 222AmmoniaHCID 866653704-Isopropoxy-3-isothiocyanato-benzenesulfonamide

生成物 1

HCID 866655834-Isopropoxy-3-thioureidobenzenesulfonamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Crude 4-isopropoxy-3-isothiocyanato-benzenesulfonamide (17.8 g, 65.2 mmol, example 2, step e) was treated with a 2 M solution of ammonia in MeOH (250 mL) and the resulting solution was stirred at room temperature for 18 h. The reaction mixture was then concentrated to about half the volume until a large amount of tan solid precipitated. The suspension was cooled to 0° C. for 30 minutes and was filtered. The solid was washed with methanol and ether to give the title compound as a cream colored solid.

後処理

  1. concentrationThe reaction mixture was then concentrated to about half the volume until a large amount of tan solid
  2. customprecipitated
  3. temperatureThe suspension was cooled to 0° C. for 30 minutes
  4. filtrationwas filtered
  5. washThe solid was washed with methanol and ether

出典と根拠

ORDレコード
ord-0f5602def9e44f86b5b52862fec149a9
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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