4-(1,4-Dioxaspiro[4.5]dec-8-ylamino)-3-methoxy-2-methylpyridine hydrochloride → 4-(4-Oxocyclohexylamino)-3-methoxy-2-methylpyridine hydrochloride

HRID 1005

반응식

HRID 1005 반응식
[ClH:1].O1[C:6]2([CH2:11][CH2:10][CH:9]([NH:12][C:13]3[CH:18]=[CH:17][N:16]=[C:15]([CH3:19])[C:14]=3[O:20][CH3:21])[CH2:8][CH2:7]2)[O:5]CC1>C(O)=O>[ClH:1].[O:5]=[C:6]1[CH2:7][CH2:8][CH:9]([NH:12][C:13]2[CH:18]=[CH:17][N:16]=[C:15]([CH3:19])[C:14]=2[O:20][CH3:21])[CH2:10][CH2:11]1

참가 물질

3

반응물 1

HCID 196940114-(1,4-Dioxaspiro[4.5]dec-8-ylamino)-3-methoxy-2-methylpyridine hydrochloride

생성물 1

HCID 196939634-(4-Oxocyclohexylamino)-3-methoxy-2-methylpyridine hydrochloride

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

27.3 g of 4-(1,4-dioxaspiro[4.5]dec-8-ylamino)-3-methoxy-2-methylpyridine hydrochloride are stirred with 400 ml of formic acid for 4 hours. The residue which remains after concentrating in vacuo is dissolved in methylene chloride and shaken with 2N NaOH. The methylene chloride phase is concentrated, the residue is dissolved in ether and the hydrochloride is precipitated by addition of ethereal HCl. 14 g=90%; m.p.: 115° to 120° C.

후처리

  1. concentrationafter concentrating in vacuo
  2. dissolutionis dissolved in methylene chloride
  3. concentrationThe methylene chloride phase is concentrated
  4. dissolutionthe residue is dissolved in ether
  5. customthe hydrochloride is precipitated by addition of ethereal HCl

출처 및 근거

ORD 기록
ord-87cd3f597261426bbf9068b66cd80964
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723450

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