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

HRID 2173381노트

반응식

HRID 2173381 반응식
C1(C(=NC2N=C(CC(O)=O)C=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH2:25][C:26]1[N:31]=[C:30]([CH2:32][C:33]([O:35][CH3:36])=[O:34])[CH:29]=[CH:28][CH:27]=1.Cl>C1COCC1.O>[NH2:25][C:26]1[N:31]=[C:30]([CH2:32][C:33]([O:35][CH3:36])=[O:34])[CH:29]=[CH:28][CH:27]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86693025Methyl (6-aminopyridin-2-yl)acetate {6-[(diphenylmethylidene)amino]pyridin-2-yl}acetate

생성물 1

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

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

methyl (6-aminopyridin-2-yl)acetate {6-[(diphenylmethylidene)amino]pyridin-2-yl}acetate (13 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. Step C: methyl [6-(1H-tetrazol-1-yl)pyridin-2-yl]acetate

후처리

  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

출처 및 근거

ORD 기록
ord-01e4cf7dc6e242ffb41f088fee507bbf
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056859B2

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