Hydrochloric Acid → 1-[2-(4-amino-1-piperidinyl)ethyl]-7-fluoro-2(1H)-quinoxalinone dihydrochloride

HRID 656943ノート

反応式

HRID 656943 の反応式
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8](=[O:28])[N:9]2[CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][CH:17]([NH:20]C(=O)OC(C)(C)C)[CH2:16][CH2:15]2)=[CH:4][CH:3]=1.[ClH:29]>CO.C(Cl)Cl.O1CCOCC1>[ClH:29].[ClH:29].[NH2:20][CH:17]1[CH2:16][CH2:15][N:14]([CH2:13][CH2:12][N:9]2[C:10]3[C:5](=[CH:4][CH:3]=[C:2]([F:1])[CH:11]=3)[N:6]=[CH:7][C:8]2=[O:28])[CH2:19][CH2:18]1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 59397942tert-butyl{1-[2-(7-fluoro-2-oxoquinoxalin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate

生成物 1

HCID 688175421-[2-(4-amino-1-piperidinyl)ethyl]-7-fluoro-2(1H)-quinoxalinone dihydrochloride

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 1,1-dimethylethyl {1-[2-(7-fluoro-2-oxo-1(2H)-quinoxalinyl)ethyl]-4-piperidinyl}carbamate (4.0 g) in dry MeOH (15 ml) and dry DCM (30 ml) was treated with 4 M hydrogen chloride in 1,4-dioxane (30 ml) and stirred at rt for 3 h. It was evaporated to dryness and the insoluble product was heated in MeOH (50 ml), cooled, filtered, washed with cold MeOH, then ether, to give a solid (3.05 g).

後処理

  1. customIt was evaporated to dryness
  2. temperaturethe insoluble product was heated in MeOH (50 ml)
  3. temperaturecooled
  4. filtrationfiltered
  5. washwashed with cold MeOH

出典と根拠

ORDレコード
ord-bc5bdbbbba6f47a1814e09d0deb45f80
出典データセット
uspto-grants-2011_12
特許番号
US08071592B2

反応ノート

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