Water → HCID 63766063, 화합물

HRID 252938

반응식

HRID 252938 반응식
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]

참가 물질

7

반응물 3

HCID 962WaterHCID 66071N-EthylethylenediamineHCID 764302-Bromothiazole

생성물 1

HCID 63766063HCID 63766063, 화합물수율 8%

시약·촉매·용매 3

HCID 23978Copper촉매HCID 62652Cuprous chloride촉매HCID 3776Isopropanol용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-82807a9b4e3f491f803518c491bf2a33
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07871999B2

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