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Sodium Hydroxide → HCID 69023783, 화합물

HRID 1007298
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HRID 1007298 반응식
[C:1]([O:5][C:6]([NH:8][C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C@@H:10]1[NH:15][C:16]1[C:25]2[C:20](=[CH:21][CH:22]=[C:23]([O:26][CH3:27])[CH:24]=2)[N:19]=[C:18]([C:28]([O:30]CC)=[O:29])[N:17]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].S([O-])(O)(=O)=O.[K+]>CO>[C:1]([O:5][C:6]([NH:8][C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C@@H:10]1[NH:15][C:16]1[C:25]2[C:20](=[CH:21][CH:22]=[C:23]([O:26][CH3:27])[CH:24]=2)[N:19]=[C:18]([C:28]([OH:30])=[O:29])[N:17]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 516920Potassium bisulfateHCID 69023628HCID 69023628, 화합물

생성물 1

HCID 69023783HCID 69023783, 화합물수율 69.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1.70 g of cis-N-tert-butoxycarbonyl-2-(2-ethoxycarbonyl-6-methoxyquinazolin-4-yl)aminocyclohexylamine in 5 mL of methanol was combined with 5 mL of a 1N aqueous solution of sodium hydroxide, and stirred at room temperature for 3 hours. After the pH was adjusted to 5 by addition of a 1N aqueous solution of potassium hydrogen sulfate to the reaction solution, which was then extracted with chloroform and dried. After the solvent was distilled off, the residue was purified by column chromatography on silica gel (chloroform:methanol=10:1) to obtain 1.10 g of the desirable compound.

후처리

  1. extractionwas then extracted with chloroform
  2. customdried
  3. distillationAfter the solvent was distilled off
  4. customthe residue was purified by column chromatography on silica gel (chloroform:methanol=10:1)

출처 및 근거

ORD 기록
ord-ed171331775b4488b2565c4fa6c23950
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06794389B2

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