Tetrahydrofuran → HCID 86605288、化合物

HRID 1348635ノート

反応式

HRID 1348635 の反応式
[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]

参加物

6

反応物 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

生成物 1

HCID 86605288HCID 86605288、化合物収率 80%

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-3716e590135c40379ae776d4ea962179
出典データセット
uspto-grants-2007_05
特許番号
US07211573B2

反応ノート

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