Hydrochloric Acid → Methyl 2-(6-aminopyridin-2-yl)acetate

HRID 1502141ノート

反応式

HRID 1502141 の反応式
C1(C(=[N:14][C:15]2[N:20]=[C:19]([CH2:21][C:22]([O-:24])=[O:23])[CH:18]=[CH:17][CH:16]=2)C2C=CC=CC=2)C=CC=CC=1.Cl.[CH2:26]1COCC1.O>>[NH2:14][C:15]1[N:20]=[C:19]([CH2:21][C:22]([O:24][CH3:26])=[O:23])[CH:18]=[CH:17][CH:16]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 21881883Oxolane--water (1/1)HCID 131734294{6-[(Diphenylmethylidene)amino]pyridin-2-yl}acetate

生成物 1

HCID 68841216Methyl 2-(6-aminopyridin-2-yl)acetate

実験手順

{6-[(diphenylmethylidene)amino]pyridin-2-yl}acetate (1.3 g, 3.93 mmol) was dissolved in 1:1 mixture of THF/water (20 mL) and treated with 4.5 mL of a 1N aqueous hydrochloric acid solution. The reaction was allowed to stir at ambient temperature for 30 minutes and then concentrated in vacuo. The crude residue was dissolved in DCM and washed with a saturated aqueous sodium bicarbonate solution. The organic layers were dried over sodium sulfate, filtered and concentrated to afford crude methyl (6-aminopyridin-2-yl)acetate which was used without further purification: LC/MS (M+H)+167.

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe crude residue was dissolved in DCM
  3. washwashed with a saturated aqueous sodium bicarbonate solution
  4. dry with materialThe organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-9b1c6dba44aa414ea260f64024ea803d
出典データセット
uspto-grants-2015_12
特許番号
US09206199B2

反応ノート

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