Potassium Carbonate → HCID 21103673、化合物

HRID 1354816ノート

反応式

HRID 1354816 の反応式
[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11](O)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].[NH2:32][C:33]1[CH:38]=[CH:37][C:36]([N+:39]([O-:41])=[O:40])=[CH:35][C:34]=1[OH:42]>C1COCC1>[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11]([NH:32][C:33]1[CH:38]=[CH:37][C:36]([N+:39]([O-:41])=[O:40])=[CH:35][C:34]=1[OH:42])=[O:12])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 49847212-Amino-5-NitrophenolHCID 9840634HCID 9840634、化合物

生成物 1

HCID 21103673HCID 21103673、化合物収率 55.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Compound 37 (1 g, 3 mmol) was dissolved in THF (100 mL). K2CO3 (2 g, 15 mmol) was added followed by 2-amino-5-nitro-phenol (693 mg, 4.5 mmol). The reaction mixture was allowed to stir at room temperature overnight. K2CO3 was filtered off though filter paper. The solvent was removed under reduced pressure. Liquid-liquid extraction was performed using CHCl3 (100 mL) and H2O (50 mL). The organic layer was dried over MgSO4. After MgSO4 was filtered off, the solvent was removed under reduced pressure. The residue was purified by flash chromatography to give compound 39 (786 mg, 55.7% isolated yield). LC-MS (ESI): m/e=471.1 [M+1]+

後処理

  1. filtrationK2CO3 was filtered off
  2. filtrationthough filter paper
  3. customThe solvent was removed under reduced pressure
  4. extractionLiquid-liquid extraction
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationAfter MgSO4 was filtered off
  7. customthe solvent was removed under reduced pressure
  8. customThe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-8eb5f4626103447eb753bebe8770a720
出典データセット
uspto-grants-2007_05
特許番号
US07223759B2

反応ノート

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