Sodium Hydroxide → HCID 70800717、化合物

HRID 2038798ノート

反応式

HRID 2038798 の反応式
[OH-].[Na+].[C:3]([O:7][C:8](=[O:17])[NH:9][C:10]1([C:14](=O)[CH3:15])[CH2:13][CH2:12][CH2:11]1)([CH3:6])([CH3:5])[CH3:4].[I:18][C:19]1[CH:20]=[C:21]([CH:26]=O)[C:22]([NH2:25])=[N:23][CH:24]=1>CCO>[C:3]([O:7][C:8](=[O:17])[NH:9][C:10]1([C:14]2[CH:15]=[CH:26][C:21]3[C:22](=[N:23][CH:24]=[C:19]([I:18])[CH:20]=3)[N:25]=2)[CH2:13][CH2:12][CH2:11]1)([CH3:6])([CH3:5])[CH3:4]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 177501772-Amino-5-iodopyridine-3-carbaldehydeHCID 67508029(1-Acetyl-cyclobutyl)-carbamic acid tert-butyl ester

生成物 1

HCID 70800717HCID 70800717、化合物収率 84%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Freshly ground NaOH (0.32 g, 7.9 mmol) was dissolved in absolute EtOH (25 mL). To this solution was added (1-acetyl-cyclobutyl)-carbamic acid tert-butyl ester (0.84 g, 3.95 mmol) and 5-iodo-2-aminopyridine-3-carboxaldehyde (0.932 g, 3.76 mmol) simultaneously as a solution in EtOH (25 mL). The reaction was allowed to stir for 72 h and the volatiles were removed in vacuo. This crude residue was diluted with CH2Cl2, absorbed onto SiO2 by removal of solvent in vacuo and purified via SiO2 flash chromatography (20-75% EtOAc-hexane) to afford the title compound as a white solid (1.34 g, 84%), m/z=366.4.

後処理

  1. customthe volatiles were removed in vacuo
  2. additionThis crude residue was diluted with CH2Cl2
  3. customabsorbed onto SiO2 by removal of solvent in vacuo
  4. custompurified via SiO2 flash chromatography (20-75% EtOAc-hexane)

出典と根拠

ORDレコード
ord-bde19b3b43b54898a1c8f7e9919e775c
出典データセット
uspto-grants-2013_11
特許番号
US08575360B2

反応ノート

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