Ethylamine → HCID 3049302, 화합물

HRID 1112726노트

반응식

HRID 1112726 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 3049302HCID 3049302, 화합물수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-57f9286ecf31489dbabdce958b8504c5
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04123541

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