Sodium Hydroxide → HCID 86722243、化合物

HRID 869398ノート

反応式

HRID 869398 の反応式
[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

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 21914786HCID 21914786、化合物HCID 86722235HCID 86722235、化合物

生成物 1

HCID 86722243HCID 86722243、化合物収率 59.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-eb61d014c8b34da986470282e432c83f
出典データセット
uspto-grants-2015_03
特許番号
US08969373B2

反応ノート

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