Water → HCID 63766063、化合物

HRID 252938

反応式

HRID 252938 の反応式
Br[C:2]1[S:3][CH:4]=[CH:5][N:6]=1.[CH2:7]([NH:9][CH2:10][CH2:11][NH2:12])[CH3:8].O>C(O)(C)C.[Cu].[Cu]Cl>[CH2:7]([N:9]([C:2]1[S:3][CH:4]=[CH:5][N:6]=1)[CH2:10][CH2:11][NH2:12])[CH3:8]

参加物

7

反応物 3

HCID 962WaterHCID 66071N-EthylethylenediamineHCID 764302-Bromothiazole

生成物 1

HCID 63766063HCID 63766063、化合物収率 8%

試薬・触媒・溶媒 3

HCID 23978Copper触媒HCID 62652Cuprous chloride触媒HCID 3776Isopropanol溶媒

反応条件

温度
70 °C

実験手順

47 mg (0.74 mmol) of copper and 225 mg (2.27 mmol) of copper(I) chloride were added to a solution of 1.35 g (15.0 mmol) of 2-bromothiazole and 9.48 ml (90.0 mmol) of N-ethylethylenediamine in isopropanol (7.5 ml). The mixture was then heated to 70° C. for 1 h. After cooling to RT, the reaction solution was poured into water and extracted with EA. The organic phase was dried over MgSO4, filtered and evaporated under a vacuum. 200 mg (1.2 mmol, 8%) of N1-ethyl-N1-(thiazol-2-yl)ethane-1,2-diamine were obtained by carrying out CC twice (i. DCE/EtOH 5:1; ii. DCE/EtOH/conc. aq. NH4OH soln. 5:1:0.06) with the residue.

後処理

  1. temperatureAfter cooling to RT
  2. extractionextracted with EA
  3. dry with materialThe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. customevaporated under a vacuum

出典と根拠

ORDレコード
ord-82807a9b4e3f491f803518c491bf2a33
出典データセット
uspto-grants-2011_01
特許番号
US07871999B2

関連ノート

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