N-Methylethylenediamine → HCID 86632288、化合物

HRID 252934

反応式

HRID 252934 の反応式
Br[C:2]1[S:3][C:4]([Br:7])=[CH:5][N:6]=1.[CH3:8][NH:9][CH2:10][CH2:11][NH2:12].ClCCCl.CCO>C(O)(C)C.[Cu].[Cu]Cl>[Br:7][C:4]1[S:3][C:2]([N:9]([CH3:8])[CH2:10][CH2:11][NH2:12])=[N:6][CH:5]=1

参加物

7

反応物 3

HCID 8014N-MethylethylenediamineHCID 3123942,5-DibromothiazoleHCID 229016121,2-Dichloroethane ethanol

生成物 1

HCID 86632288HCID 86632288、化合物収率 36.6%

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

15 mg (0.24 mmol) of copper and 68 mg (0.69 mmol) of copper(I) chloride were added to a solution of 1.0 g (4.1 mmol) of 2,5-dibromothiazole and 2.2 ml (24.7 mmol) of N-methylethylenediamine in isopropanol (2.3 ml). The mixture was then heated to 70° C. for 1 h. After cooling to RT, filtration through silica gel was carried out and the filtrate was evaporated under a vacuum. 348 mg (1.5 mmol, 36%) of N1-(5-bromothiazol-2-yl)-N1-methylethane-1,2-diamine were obtained by CC (DCE/EtOH/conc. aq. NH4—OH soln. 5:1:0.06) with the residue.

後処理

  1. temperatureAfter cooling to RT
  2. filtrationfiltration through silica gel
  3. customthe filtrate was evaporated under a vacuum

出典と根拠

ORDレコード
ord-854ce2e82f524dfc9e68a65540978a77
出典データセット
uspto-grants-2011_01
特許番号
US07871999B2

関連ノート

読み込み中…