Hydrochloric Acid → HCID 14126765、化合物

HRID 476907ノート

反応式

HRID 476907 の反応式
Cl.[CH3:2][NH:3][CH2:4][CH2:5][Cl:6].[SH:7][C:8]1[N:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]2=[N:10][N:9]=1.C(N(CC)CC)C.Cl>C(O)C.C(OCC)C.CC(C)=O.C(OCC)C>[ClH:6].[CH3:2][NH:3][CH2:4][CH2:5][S:7][C:8]1[N:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]2=[N:10][N:9]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 3028223Ethanamine, 2-chloro-N-methyl-, hydrochloride (1:1)HCID 178527925HCID 178527925、化合物

生成物 1

HCID 14126765HCID 14126765、化合物収率 38.9%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒HCID 21584533Acetone diethylether溶媒

実験手順

A solution of 18 g of N-methyl-2-chloroethylamine hydrochloride, 20 g of 3-mercapto-1,2,4-triazolo(4,3-a)pyridine and 40 ml of triethylamine in 150 ml of ethanol is heated under reflux for 2 hours. After evaporation, the residue is taken up in water, 0.1N sodium hydroxide is added and extraction is carried out with chloroform. The chloroform phase is washed with water, dried over sodium sulfate and evaporated to dryness. The residue obtained is dissolved in an ethyl ether/acetone mixture and the solution is acidified by the addition of a solution of ethyl ether saturated with hydrogen chloride gas. The precipitate formed is filtered off, washed with ether and dried to give 12.6 g of 3-[2-(methylamino)ethylmercapto]-1,2,4-triazolo(4,3-a)pyridine hydrochloride in the form of crystals melting at 195°-7° C.

後処理

  1. temperatureunder reflux for 2 hours
  2. customAfter evaporation
  3. addition0.1N sodium hydroxide is added
  4. extractionextraction
  5. washThe chloroform phase is washed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated to dryness
  8. customThe residue obtained
  9. customThe precipitate formed
  10. filtrationis filtered off
  11. washwashed with ether
  12. customdried

出典と根拠

ORDレコード
ord-0e5859de25f346cba5278d7a7ea35075
出典データセット
uspto-grants-1989_12
特許番号
US04886805

反応ノート

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