반응식
[NH2:1][C:2]1[N:7]=[C:6]([C:8](O)=O)[CH:5]=[CH:4][CH:3]=1.[NH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[NH2:18].[OH-].[Na+]>>[N:7]1[CH:2]=[CH:3][CH:4]=[CH:5][C:6]=1[C:3]1[C:2]([NH2:1])=[N:7][C:6]([C:8]2[NH:18][C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[N:11]=2)=[CH:5][CH:4]=1참가 물질
4
실험 절차
A suspension of 6-aminopyridine-2-carboxylic acid (1.12 g, 8.2 mmol) with 1,2-diaminobenzene (1.77 mg,16.4 mmol) was heated in 8 mL of PPA at 180 degree for 2 h. The reaction mixture was poured into 250 mL of ice-water and neutralized with 2 N NaOH (chilled) while vigorously stirred. The resulting precipitate was filtered to collect an off-white solid, which was washed with 20 mL warm water, dried and purified by chromatography using a 9:1 mixture of CH2Cl2 to MeOH (MS, M++H=211).
후처리
- temperaturewas heated in 8 mL of PPA at 180 degree for 2 h
- filtrationThe resulting precipitate was filtered
- customto collect an off-white solid, which
- washwas washed with 20 mL
- temperaturewarm water
- customdried
- custompurified by chromatography
- additiona 9:1 mixture of CH2Cl2 to MeOH (MS, M++H=211)
출처 및 근거
- ORD 기록
- ord-d766fec0940c48e7ad24d38f41bb1b34
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08093401B2
연결된 노트
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