Hydrochloric Acid → N,N-dimethyl-N'-(3-cyano-5-ethoxycarbonylthieno[3,2-b]thien-2-yl)formamidine

HRID 1905460ノート

反応式

HRID 1905460 の反応式
[C:1]([O:5][CH2:6][CH3:7])(=[O:4])[CH2:2][SH:3].[CH3:8][N:9]([CH3:22])[CH:10]=[N:11][C:12]1[S:13][C:14]([CH:20]=O)=[C:15](Cl)[C:16]=1[C:17]#[N:18].C(=O)([O-])[O-].[K+].[K+].Cl>O.CN(C)C=O>[CH3:22][N:9]([CH3:8])[CH:10]=[N:11][C:12]1[S:13][C:14]2[CH:20]=[C:2]([C:1]([O:5][CH2:6][CH3:7])=[O:4])[S:3][C:15]=2[C:16]=1[C:17]#[N:18]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 12185Ethyl ThioglycolateHCID 54382946N'-(4-chloro-3-cyano-5-formyl-2-thienyl)-N,N-dimethylformamidine

生成物 1

HCID 68115437N,N-dimethyl-N'-(3-cyano-5-ethoxycarbonylthieno[3,2-b]thien-2-yl)formamidine収率 93%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

120 parts of ethyl thioglycolate were added to a mixture of 241.5 parts of N,N-dimethyl-N'-(4-chloro-3-cyano-5-formylthien-2-yl)formamidine, 138 parts of potassium carbonate and 1,400 parts of N,N-dimethylformamide. After the slightly exothermic reaction had died down, the reaction mixture was stirred at 50° C. for 2 hours. 1,000 parts of ice, 1,000 parts of water and 150 parts of concentrated hydrochloric acid were then added. The precipitate was filtered off with suction, washed with water and dried. This gave 284 parts (93% of theory) of N,N-dimethyl-N'-(3-cyano-5-ethoxycarbonylthieno[3,2-b]thien-2-yl)formamidine.

後処理

  1. customAfter the slightly exothermic reaction
  2. filtrationThe precipitate was filtered off with suction
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-d56900313ebd4ca9ab8198c03269c71f
出典データセット
uspto-grants-1989_06
特許番号
US04843153

反応ノート

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