Tetrahydrofuran → HCID 86605291, 화합물

HRID 1348656노트

반응식

HRID 1348656 반응식
[CH2:1]([O:3][C:4](=[O:11])[C:5]([OH:10])([CH3:9])[C:6]([OH:8])=O)[CH3:2].O1CCCC1.Cl.[F:18][C:19]([F:24])([F:23])[CH2:20][CH2:21][NH2:22].Cl.CN(C)CCCN=C=NCC.C(N(CC)C(C)C)(C)C>>[CH2:1]([O:3][C:4](=[O:11])[C:5]([OH:10])([CH3:9])[C:6]([NH:22][CH2:21][CH2:20][C:19]([F:24])([F:23])[F:18])=[O:8])[CH3:2]

참가 물질

6

반응물 5

HCID 8028TetrahydrofuranHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 13396337Propanedioic acid, 2-hydroxy-2-methyl-, 1-ethyl esterHCID 252105053,3,3-Trifluoropropylamine hydrochloride

생성물 1

HCID 86605291HCID 86605291, 화합물수율 94%

실험 절차

To a solution of 2.00 g (8.51 mmol) 2-hydroxy-2-methyl-malonic acid monoethyl ester in 60 ml of tetrahydrofuran 1.27 g (8.51 mmol) of 3,3,3-trifluoropropylamine hydrochloride, 1.67 g (8.51 mmol) of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride, 1.17 g (8.51 mmol) of 1-hydroxybenzotrizole hydrate and 4.46 ml (25.5 mmol) of N,N-diisopropyl-ethylamine were added. The mixture was stirred at room temperature for 18 h. Silicagel was added and the solvent was removed by distillation. The residue was purified by chromatography on silicagel dichloromethane/methanol 7:3 to yield 2.33 g (94%) of the title compound, MS m/e (%): 258.1 (M+H+, 100).

후처리

  1. additionSilicagel was added
  2. customthe solvent was removed by distillation
  3. customThe residue was purified by chromatography on silicagel dichloromethane/methanol 7:3

출처 및 근거

ORD 기록
ord-cf011bfecebe4d52927535f578a763df
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211573B2

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