Hydrochloric Acid → 3-(piperidin-4-yl)-1,6-naphthyridin-2(1H)-one

HRID 132356

반응식

HRID 132356 반응식
Cl.O[CH:3]([C:22]1[CH:23]=[N:24][CH:25]=[CH:26][C:27]=1[NH:28][C:29](=[O:34])C(C)(C)C)[CH:4]([CH:9]1[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]1)C(OC)=O>O>[NH:12]1[CH2:11][CH2:10][CH:9]([C:4]2[C:29](=[O:34])[NH:28][C:27]3[C:22]([CH:3]=2)=[CH:23][N:24]=[CH:25][CH:26]=3)[CH2:14][CH2:13]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59732007tert-Butyl 4-(1-hydroxy-3-methoxy-3-oxo-1-(4-pivalamidopyridin-3-yl)propan-2-yl)piperidine-1-carboxylate

생성물 1

HCID 597319443-(piperidin-4-yl)-1,6-naphthyridin-2(1H)-one수율 77%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Concentrated hydrochloric acid (8.0 mL, 97 mmol) was added with stirring to a mixture of tert-butyl 4-(1-hydroxy-3-methoxy-3-oxo-1-(4-pivalamidopyridin-3-yl)propan-2-yl)piperidine-1-carboxylate (1.2 g, 2.6 mmol) and water (24 mL). Reaction was heated to reflux and held for 14 hours. Mixture was concentrated in vacuo. Residue was treated with acetonitrile (70 mL) and then concentrated in vacuo. Residue was crystallized from ethanol. Title compound was obtained as white solid in 77% yield. (M+H)+=230.1.

후처리

  1. customReaction
  2. temperaturewas heated
  3. temperatureto reflux
  4. concentrationMixture was concentrated in vacuo
  5. additionResidue was treated with acetonitrile (70 mL)
  6. concentrationconcentrated in vacuo
  7. customResidue was crystallized from ethanol

출처 및 근거

ORD 기록
ord-b1320bd028ea441c8a46e54e81db2eb5
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384931B2

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