Tetrahydrofuran → HCID 86605288, 화합물

HRID 1348635노트

반응식

HRID 1348635 반응식
[CH2:1]([O:3][C:4](=[O:11])[C:5]([OH:10])([CH3:9])[C:6]([OH:8])=O)[CH3:2].O1CCCC1.[F:17][C:18]([F:25])([C:21]([F:24])([F:23])[F:22])[CH2:19][NH2:20].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:20][CH2:19][C:18]([F:25])([F:17])[C:21]([F:24])([F:23])[F:22])=[O:8])[CH3:2]

참가 물질

6

반응물 5

HCID 8028TetrahydrofuranHCID 790022,2,3,3,3-PentafluoropropylamineHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 13396337Propanedioic acid, 2-hydroxy-2-methyl-, 1-ethyl ester

생성물 1

HCID 86605288HCID 86605288, 화합물수율 80%

실험 절차

To a solution of 2.08 g (12.8 mmol) 2-hydroxy-2-methyl-malonic acid monoethyl ester in 50 ml of tetrahydrofuran 1.39 g (12.8 mmol) of 2,2,3,3,3-pentafluoropropylamine, 2.51 g (12.8 mmol) of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride, 1.77 g (12.8 mmol) of 1-hydroxybenzotrizole hydrate and 4.48 ml (25.7 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 (ethyl acetate/heptane=0:100 to 50:50) to yield 3.01 g (80%) of the title compound as white solid, MS m/e (%): 292.1 (M−H+, 100).

후처리

  1. additionSilicagel was added
  2. customthe solvent was removed by distillation
  3. customThe residue was purified by chromatography on silicagel (ethyl acetate/heptane=0:100 to 50:50)

출처 및 근거

ORD 기록
ord-3716e590135c40379ae776d4ea962179
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211573B2

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