Pyridine → HCID 69063936, 화합물

HRID 2110015노트

반응식

HRID 2110015 반응식
[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

참가 물질

5

반응물 3

HCID 1049Pyridine2회HCID 155402-Nitrobenzenesulfonyl chloride2회HCID 18621647Methyl 3-amino-4-[(tert-butoxycarbonyl)amino]benzoate

생성물 1

HCID 69063936HCID 69063936, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8f950a557c6748329d431bf03c815f56
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517875B2

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