Thiophosgene → 4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylisothiocyanate

HRID 33760

反応式

HRID 33760 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][C:6]=1[F:12].C(=O)(O)[O-].[Na+].[C:23](Cl)(Cl)=[S:24]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]=[C:23]=[S:24])=[CH:7][C:6]=1[F:12]

参加物

5

反応物 3

HCID 10040ThiophosgeneHCID 516892Sodium BicarbonateHCID 289727064-(2,5-Dichlorophenoxy)-3-fluoroaniline

生成物 1

HCID 597976634-(2,5-Dichloro-phenoxy)-3-fluoro-phenylisothiocyanate収率 97.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylamine (1.36 g, 5 mmol) was dissolved in 150 ml of chloroform and 100 ml of saturated aqueous sodium bicarbonate was added. To this biphasic mixture was added dropwise a solution of thiophosgene (0.39 ml, 5 mmol) in 30 ml of chloroform at room temperature with vigorous stirring. The mixture was stirred vigorously for 1 hour at room temperature. The bottom layer of the mixture was separated, and the aqueous layer was extracted twice with CHCl3. The combined organic solution was washed with water, dried over Mg2SO4 and evaporated to give 1.53 g (97.4%) of crude product used for next step without further purification.

後処理

  1. customThe bottom layer of the mixture was separated
  2. extractionthe aqueous layer was extracted twice with CHCl3
  3. washThe combined organic solution was washed with water
  4. dry with materialdried over Mg2SO4
  5. customevaporated

出典と根拠

ORDレコード
ord-b997bf5941b9465ca8966a1a87240e14
出典データセット
uspto-grants-2008_09
特許番号
US07429667B2

関連ノート

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