Sodium Hydroxide → HCID 70800717, 화합물

HRID 2038798노트

반응식

HRID 2038798 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 70800717HCID 70800717, 화합물수율 84%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-bde19b3b43b54898a1c8f7e9919e775c
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08575360B2

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