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

HRID 477937
ノート
印刷プレビュー

反応式

HRID 477937 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 159141297-Chlorothieno[2,3-c]pyridineHCID 53442613Sodium hydrogen sulfide hydrate2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

(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°.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-a6fbb8e7559242bcb4790b03e27079aa
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04889848

反応ノート

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