Tetrahydrofuran → HCID 86605291、化合物

HRID 1348656ノート

反応式

HRID 1348656 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.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]

参加物

6

反応物 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

生成物 1

HCID 86605291HCID 86605291、化合物収率 94%

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-cf011bfecebe4d52927535f578a763df
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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