Triethylamine → HCID 13932886, 화합물

HRID 256151

반응식

HRID 256151 반응식
Cl.[CH3:2][O:3][C:4](=[O:10])[C@@H:5]1[CH2:9][CH2:8][CH2:7][NH:6]1.[O:11]([CH2:18][CH2:19][C:20](O)=[O:21])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(N(CC)CC)C.CCN=C=NCCCN(C)C.Cl>C(Cl)Cl>[CH3:2][O:3][C:4](=[O:10])[C@@H:5]1[CH2:9][CH2:8][CH2:7][N:6]1[C:20](=[O:21])[CH2:19][CH2:18][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 815963-Phenoxypropionic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2733200methyl L-prolinate hydrochloride

생성물 1

HCID 13932886HCID 13932886, 화합물수율 65.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Proline methyl ester hydrochloride (3.4 g), 3-phenoxypropionic acid (3.4 g) and triethylamine (2.8 ml) were suspended in dry methylene chloride (30 ml). To the cooled suspension, WSCD HCl (N-ethyl-N',N'-dimethylaminopropyl-carbodiimide hydrochloride) (3.9 g) was added. Under cooling, the mixture was stirred for 1 hour, and after allowing the mixture to warm to room temperature, it was again stirred for 18 horus. The stirred mixture was washed successively with water, 1N HCl, water, saturated aqueous sodium bicarbonate and brine. After drying over anhydrous magnesium sulfate, the solvent was distilled off under vacuum. The resulting crude product was purified by medium-pressure liquid column chromatography on silica gel (solvent: chloroform) to obtain the end compound as an oil (3.7 g).

후처리

  1. temperatureUnder cooling
  2. stirringit was again stirred for 18 horus
  3. washThe stirred mixture was washed successively with water, 1N HCl, water, saturated aqueous sodium bicarbonate and brine
  4. dry with materialAfter drying over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under vacuum
  6. customThe resulting crude product was purified by medium-pressure liquid column chromatography on silica gel (solvent: chloroform)

출처 및 근거

ORD 기록
ord-808e90378d7b40a881a80eac832fb315
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04701465

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