Thiophosgene → Methyl 4-isothiocyanatothiophene-3-carboxylate

HRID 1978862ノート

反応式

HRID 1978862 の反応式
Cl.[NH2:2][C:3]1[C:4]([C:8]([O:10][CH3:11])=[O:9])=[CH:5][S:6][CH:7]=1.[C:12](Cl)(Cl)=[S:13].C(=O)(O)[O-].[Na+]>O.ClCCl>[N:2]([C:3]1[C:4]([C:8]([O:10][CH3:11])=[O:9])=[CH:5][S:6][CH:7]=1)=[C:12]=[S:13]

参加物

6

反応物 3

HCID 10040ThiophosgeneHCID 516892Sodium BicarbonateHCID 2777609Methyl 4-aminothiophene-3-carboxylate Hydrochloride

生成物 1

HCID 23259576Methyl 4-isothiocyanatothiophene-3-carboxylate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

19.4 g of methyl 4-aminothiophen-3-carboxylate hydrochloride were added to a suspension of 7.7 ml of thiophosgene and 18.5 g of sodium bicarbonate in 70 ml of water and 200 ml of dichloromethane at room temperature in the course of 30 minutes, and stirring was carried out for 1 hour at room temperature. After separation of the phases, the aqueous phase was extracted once with dichloromethane and the combined organic phases were washed once with water, dried over sodium sulfate and evaporated down.

後処理

  1. customAfter separation of the phases
  2. extractionthe aqueous phase was extracted once with dichloromethane
  3. washthe combined organic phases were washed once with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated down

出典と根拠

ORDレコード
ord-ac2311a495f74cd18536f858cc4d5028
出典データセット
uspto-grants-2001_05
特許番号
US06239074B1

反応ノート

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