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Hydrochloric Acid → Thieno[2,3-c]pyridine-7(6H)-thione

HRID 477937
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반응식

HRID 477937 반응식
Cl[C:2]1[N:3]=[CH:4][CH:5]=[C:6]2[CH:10]=[CH:9][S:8][C:7]=12.O.[SH2:12].[Na].Cl>CN(C)C=O>[S:8]1[C:7]2[C:2](=[S:12])[NH:3][CH:4]=[CH:5][C:6]=2[CH:10]=[CH:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 159141297-Chlorothieno[2,3-c]pyridineHCID 53442613Sodium hydrogen sulfide hydrate2회

생성물 1

HCID 14666714Thieno[2,3-c]pyridine-7(6H)-thione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

(adc) 4.85 g of 7-chloro-thieno[2,3-c]pyridine were dissolved in 15 ml of dimethylformamide and 3.18 g of sodium hydrogen sulfide monohydrate were added under argon. The mixture was heated to 110°-115° for one hour, an additional 1.06 g of sodium hydrogen sulfide monohydrate were added and the mixture was held at the temperature indicated above for an additional hour. The mixture was poured on to 150 ml of ice-water and acidified with 1N aqueous hydrochloric acid solution. After stirring at 2° for a short time, the yellowish crystals were removed by filtration. After recrystallization from a toluene/ethyl acetate mixture, there was obtained pure thieno[2,3-c]pyridine-7(6H)-thione, m.p. 187°-189°.

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후처리

  1. temperatureThe mixture was heated to 110°-115° for one hour
  2. customthe yellowish crystals were removed by filtration
  3. customAfter recrystallization from a toluene/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-a6fbb8e7559242bcb4790b03e27079aa
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04889848

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