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Propargylamine → HCID 20165017、化合物

HRID 255876
ノート
印刷プレビュー

反応式

HRID 255876 の反応式
[CH2:1]([NH2:4])[C:2]#[CH:3].Cl.Cl[CH2:7][CH2:8][NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=1>C(Cl)Cl>[CH2:1]([NH:4][CH2:7][CH2:8][NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:17])([F:18])[F:19])[CH:11]=1)[C:2]#[CH:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 239041PropargylamineHCID 20165021HCID 20165021、化合物

生成物 1

HCID 20165017HCID 20165017、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

16.5 g of (0.3 mol) of propargylamine were dissolved in 100 ml of absolute methylene chloride, and the solution was admixed at room temperature in portions with the N-(2-chloro-ethyl)-3-(trifluoromethyl)-aniline hydrochloride obtained in step 3.1. While monitoring by chromatography, the mixture was heated until the reaction had gone to completion. After the reaction had ended, the reaction solution were extracted with the calculated quantity of sodium carbonate solution. After drying with sodium sulfate, the organic phase was evaporated under reduced pressure. The oily base thus obtained was used as such in the next step. (If this product contains significant impurities, it is advisable to recrystallize as its dihydrochloride).

後処理

  1. temperaturethe mixture was heated until the reaction
  2. extractionthe reaction solution were extracted with the calculated quantity of sodium carbonate solution
  3. dry with materialAfter drying with sodium sulfate
  4. customthe organic phase was evaporated under reduced pressure
  5. customThe oily base thus obtained
  6. customto recrystallize as its dihydrochloride)

出典と根拠

ORDレコード
ord-fda01db0b2734bb28c5b39c924e606d5
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04699910

反応ノート

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