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

HRID 1005

反応式

HRID 1005 の反応式
[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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-87cd3f597261426bbf9068b66cd80964
出典データセット
uspto-grants-1998_03
特許番号
US05723450

関連ノート

読み込み中…