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Ethyl trifluoroacetate → HCID 67387617、化合物

HRID 1468588
ノート
印刷プレビュー

反応式

HRID 1468588 の反応式
[F:1][C:2]([F:9])([F:8])[C:3](OCC)=O.O.[NH2:11][NH2:12].C(S[C:16]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[N:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)C>C(O)CCC>[C:24]1([C:16]2[N:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:3]([C:2]([F:1])([F:8])[F:9])=[N:12][N:11]=2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
参加物反応条件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 9794Ethyl trifluoroacetateHCID 24654Hydrazine hydrate (1:1)HCID 13377974Ethyl N-phenylbenzenecarboximidothioate

生成物 1

HCID 67387617HCID 67387617、化合物収率 26%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
0 °C

実験手順

First, 1.8 g of ethyl trifluoroacetate and 50 mL of 1-butanol were put in a three-neck flask, and the air in the flask was replaced by nitrogen. After that, the mixture was stirred at 0° C. for 10 minutes, and 0.397 g of hydrazine monohydrate was dripped to the mixed solution. This mixed solution was stirred at 0° C. for 20 minutes, and then stirred at room temperature for 1 hour to be reacted. After the reaction, 3.0 g of N-[(ethylsulfanyl)phenylmethylidene]aniline was further added to the mixed solution, and the solution was heated and stirred at 120° C. for 5 hours to be reacted. The mixed solution after the reaction was cooled down to room temperature and filtered, so that filtrate was obtained. The obtained filtrate was concentrated to give a solid. This solid was washed with hexane, so that the triazole derivative HCF3ptz was prepared (yield: 26%). The synthesis scheme of Step 1 is shown by (a-2).

後処理

  1. stirringThis mixed solution was stirred at 0° C. for 20 minutes
  2. stirringstirred at room temperature for 1 hour
  3. customto be reacted
  4. additionwas further added to the mixed solution
  5. temperaturethe solution was heated
  6. stirringstirred at 120° C. for 5 hours
  7. customto be reacted
  8. temperatureThe mixed solution after the reaction was cooled down to room temperature
  9. filtrationfiltered, so that filtrate
  10. customwas obtained
  11. concentrationThe obtained filtrate was concentrated
  12. customto give a solid
  13. washThis solid was washed with hexane, so that the triazole derivative HCF3ptz
  14. customwas prepared (yield: 26%)
  15. customThe synthesis scheme of Step 1

出典と根拠

ORDレコード
ord-b70c02b5970048e48da12860c0563424
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09005773B2

反応ノート

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