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2,3-Diaminopyridine → Benzyl (2-aminopyridin-3-yl)carbamate

HRID 547382
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반응식

HRID 547382 반응식
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH2:9]([O:16][C:17](Cl)=[O:18])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>O1CCCC1.N1C=CC=CC=1>[NH2:1][C:2]1[C:7]([NH:8][C:17](=[O:18])[O:16][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][CH:5]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 99562,3-DiaminopyridineHCID 10387Benzyl chloroformate

생성물 1

HCID 13451701Benzyl (2-aminopyridin-3-yl)carbamate

시약·촉매·용매 1

HCID 16069498Pyridine tetrahydrofuran용매

실험 절차

To a solution of 2,3-diaminopyridine in tetrahydrofuran/pyridine (10/1) at 0° C. benzylchloroformate was added dropwise. The suspension was stirred at room temperature and after 2 hours partitioned between water and EtOAc. The organic phase was separated and the aqueous phase was extracted with EtOAc. The combined organic phases were dried over sodium sulfate and the filtrate concentrated to dryness under reduced pressure. To the residue was added Et2O-MeOH and the solid was filtered.

후처리

  1. custompartitioned between water and EtOAc
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with EtOAc
  4. dry with materialThe combined organic phases were dried over sodium sulfate
  5. concentrationthe filtrate concentrated to dryness under reduced pressure
  6. additionTo the residue was added Et2O-MeOH
  7. filtrationthe solid was filtered

출처 및 근거

ORD 기록
ord-4b96f569b809458f94b63f6d610ec9c0
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07939537B2

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