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

HRID 547382
ノート
印刷プレビュー

反応式

HRID 547382 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 99562,3-DiaminopyridineHCID 10387Benzyl chloroformate

生成物 1

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

試薬・触媒・溶媒 1

HCID 16069498Pyridine tetrahydrofuran溶媒

実験手順

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.

後処理

このページの内容参加物実験手順後処理出典と根拠反応ノート
  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

出典と根拠

ORDレコード
ord-4b96f569b809458f94b63f6d610ec9c0
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07939537B2

反応ノート

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