Sodium Hydroxide → HCID 86722243, 화합물

HRID 869398노트

반응식

HRID 869398 반응식
[C:1]([C:4]1[O:5][C:6]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([Cl:16])[C:7]=2[C:8]=1[NH2:9])(=[O:3])[CH3:2].[CH:17]([C:19]1[N:20]=[C:21]([NH:24][C:25](=[O:29])[CH:26]([CH3:28])[CH3:27])[S:22][CH:23]=1)=O.[OH-].[Na+]>C1COCC1>[NH2:9][C:8]1[C:7]2[C:10]([Cl:16])=[C:11]([O:14][CH3:15])[CH:12]=[CH:13][C:6]=2[O:5][C:4]=1[C:1](=[O:3])[CH:2]=[CH:17][C:19]1[N:20]=[C:21]([NH:24][C:25](=[O:29])[CH:26]([CH3:27])[CH3:28])[S:22][CH:23]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 21914786HCID 21914786, 화합물HCID 86722235HCID 86722235, 화합물

생성물 1

HCID 86722243HCID 86722243, 화합물수율 59.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

7G (2.5 g, 10.4 mmol) was dissolved in THF (25 mL). To the solution was added 11D (2.4 g, 1.2 eq, 12.5 mmol), followed by crushed NaOH powder (0.8 g, 2 eq, 20.8 mmol). The reaction mixture was stirred at room temperature for about 1 hour and the solution was getting darker. After reaction completed, the mixture was poured into ice-water under stirring. The solids were collected by filtration, dried and purified by column chromatography on silica gel to give 2.6 g of pure product 11E.

후처리

  1. customAfter reaction
  2. stirringunder stirring
  3. filtrationThe solids were collected by filtration
  4. customdried
  5. custompurified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-eb61d014c8b34da986470282e432c83f
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969373B2

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