Thiophosgene → 4-Methylsulfonylphenylisothiocyanate

HRID 30161

反応式

HRID 30161 の反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][CH:6]=1)(=[O:4])=[O:3].[C:12](Cl)(Cl)=[S:13]>O.Cl>[N:11]([C:8]1[CH:9]=[CH:10][C:5]([S:2]([CH3:1])(=[O:3])=[O:4])=[CH:6][CH:7]=1)=[C:12]=[S:13]

参加物

5

反応物 2

HCID 10040ThiophosgeneHCID 796174-(Methylsulfonyl)aniline

生成物 1

HCID 150782064-Methylsulfonylphenylisothiocyanate収率 85.2%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

A solution of 4-methanesulfonylphenylamine (2.4 g, 14 mmol) was dissolved in a mixture of water (30 mL) and hydrochloric acid (9 mL, 37%). This was treated drop wise at room temperature with thiophosgene (1.5 g, 13.2 mmol) with good stirring. After 1 h, the suspension was filtered, washed with water and dried over P2O5 to give 2.4 g (85% yield) of 1-isothiocyanato4-methanesulfonylbenzene. 1H NMR (CDCl3), 300 MHz δ3.09 (s, 3H, CH3), 7.41(d, 2H, Aromatic), 7.98 (d, 2H, Aromatic).

後処理

  1. filtrationthe suspension was filtered
  2. washwashed with water
  3. dry with materialdried over P2O5

出典と根拠

ORDレコード
ord-e092182de60b48639366dedfe02287ff
出典データセット
uspto-grants-2008_09
特許番号
US07423053B2

関連ノート

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