Pyridine → HCID 69063936、化合物

HRID 2110015ノート

反応式

HRID 2110015 の反応式
[CH3:1][O:2][C:3](=[O:19])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])=[C:6]([NH2:18])[CH:5]=1.N1C=CC=CC=1.[N+:26]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=1[S:35](Cl)(=[O:37])=[O:36])([O-:28])=[O:27]>ClCCl>[CH3:1][O:2][C:3](=[O:19])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([O:13][C:14]([CH3:16])([CH3:15])[CH3:17])=[O:12])=[C:6]([NH:18][S:35]([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][C:29]=2[N+:26]([O-:28])=[O:27])(=[O:36])=[O:37])[CH:5]=1

参加物

5

反応物 3

HCID 1049Pyridine2 回HCID 155402-Nitrobenzenesulfonyl chloride2 回HCID 18621647Methyl 3-amino-4-[(tert-butoxycarbonyl)amino]benzoate

生成物 1

HCID 69063936HCID 69063936、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

After dissolving 3-amino-4-tert-butoxycarbonylaminobenzoic acid methyl ester (817.3 mg, 3.07 mmol) in dichloromethane (10 ml), pyridine (0.373 ml, 4.60 mmol) and 2-nitrobenzenesulfonyl chloride (815 mg, 3.68 mmol) were added in an ice bath, and the mixture was stirred at room temperature for 4 hours. Pyridine (0.050 ml) and 2-nitrobenzenesulfonyl chloride (135 mg) were added, and stirring was continued for 2 hours. The reaction mixture was concentrated under reduced pressure, water (30 ml) was added, and then extraction was performed with ethyl acetate (20 ml×3 times). The obtained organic layer was washed with saturated brine and then dried over anhydrous magnesium sulfate. After concentration under reduced pressure, the crystallized residue was suspended in n-hexane-ethyl acetate (4:1), filtered, and dried to obtain 4-tert-butoxycarbonylamino-3-(2-nitro-benzenesulfonylamino)-benzoic acid methyl ester. The compound was identified by LC-MS.

後処理

  1. additionwere added in an ice bath
  2. stirringstirring
  3. waitwas continued for 2 hours
  4. concentrationThe reaction mixture was concentrated under reduced pressure, water (30 ml)
  5. additionwas added
  6. extractionextraction
  7. washThe obtained organic layer was washed with saturated brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationAfter concentration under reduced pressure
  10. filtrationfiltered
  11. customdried

出典と根拠

ORDレコード
ord-8f950a557c6748329d431bf03c815f56
出典データセット
uspto-grants-2009_04
特許番号
US07517875B2

反応ノート

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