Ethylamine → HCID 3049302、化合物

HRID 866851ノート

反応式

HRID 866851 の反応式
Cl[CH2:2][C:3]1[O:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)=[CH:6][N:7]=1.[CH2:15]([NH2:17])[CH3:16]>C(O)C>[CH2:15]([NH:17][CH2:2][C:3]1[O:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)=[CH:6][N:7]=1)[CH3:16]

参加物

4

反応物 2

HCID 6341EthylamineHCID 7369662-(Chloromethyl)-5-(4-chlorophenyl)-1,3-oxazole

生成物 1

HCID 3049302HCID 3049302、化合物収率 88%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2.3 g of 2-chloromethyl-5-(4-chlorophenyl) oxazole in 50 ml of ethanol was added 3.2 g of 70% ethylamine aqueous solution, and the resultant solution was allowed to stand at room temperature overnight. At the end of this time, the solvent and the excess ethylamine were distilled off under reduced pressure, and then 30 ml of water, 10 ml of 2N NaOH solution and 50 ml of chloroform were added. The chloroform layer was separated and the aqueous layer was extracted twice with 30 ml of chloroform. The combined chloroform layer was dried over anhydrous sodium sulfate, and the solvent was removed in vacuo to give 2.1 g of crude 2-ethylaminomethyl-5-(4-chlorophenyl) oxazole. This was dissolved in 15 ml of ethanol, and 5 ml of ethanolic saturated hydrogen chloride solution was added. Evaporation of the solvent followed by recrystallization from ethanol afforded 2.0 g (73 percent) of 2-ethylaminomethyl-5-(4-chlorophenyl) oxazole hydrochloride, M. P. 194°-6° C.

後処理

  1. distillationAt the end of this time, the solvent and the excess ethylamine were distilled off under reduced pressure
  2. addition30 ml of water, 10 ml of 2N NaOH solution and 50 ml of chloroform were added
  3. customThe chloroform layer was separated
  4. extractionthe aqueous layer was extracted twice with 30 ml of chloroform
  5. dry with materialThe combined chloroform layer was dried over anhydrous sodium sulfate
  6. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-74554bcf51c7400da6e7163bf67b74da
出典データセット
uspto-grants-1978_07
特許番号
US04101660

反応ノート

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