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p-Toluenesulfonic acid → Methyl 9-{[(benzyloxy)carbonyl]amino}-3-hydroxy-4-oxo-4-H-pyrido[1,2-a]pyrimidine-2-carboxylate

HRID 547384
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HRID 547384 반응식
[NH2:1][C:2]1[C:7]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:6][CH:5]=[CH:4][N+:3]=1[O-].[CH3:20][O:21][C:22]([C:24]#[C:25][C:26]([O:28]C)=O)=[O:23].C1(C)C=CC(S(O)(=O)=[O:37])=CC=1>C(Cl)(Cl)Cl>[CH2:11]([O:10][C:9]([NH:8][C:7]1[C:2]2=[N:1][C:24]([C:22]([O:21][CH3:20])=[O:23])=[C:25]([OH:37])[C:26](=[O:28])[N:3]2[CH:4]=[CH:5][CH:6]=1)=[O:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 12980Dimethyl acetylenedicarboxylateHCID 178508042HCID 178508042, 화합물

생성물 1

HCID 54751204Methyl 9-{[(benzyloxy)carbonyl]amino}-3-hydroxy-4-oxo-4-H-pyrido[1,2-a]pyrimidine-2-carboxylate

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
70 °C

실험 절차

To a solution of benzyl (2-amino-1-oxidopyridin-3-yl)carbamate in chloroform (filtered over alumina) was added DMAD and p-toluenesulfonic acid. The suspension was stirred at 70° C. for 12 hours. The solvent was then removed under reduced pressure and to the residue was added MeOH. The solid was filtered, washed with MeOH and dried under vacuum.

후처리

  1. customThe solvent was then removed under reduced pressure and to the residue
  2. additionwas added MeOH
  3. filtrationThe solid was filtered
  4. washwashed with MeOH
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-a538fd7e89ea4122a0ef860d60e13e5c
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07939537B2

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