Thiophosgene → Methyl 4-isothiocyanatothiophene-3-carboxylate

HRID 1978862노트

반응식

HRID 1978862 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

HCID 23259576Methyl 4-isothiocyanatothiophene-3-carboxylate

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ac2311a495f74cd18536f858cc4d5028
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06239074B1

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