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Hydrochloric Acid → 4,5-dihydro-4-[2-(piperidin-4-yl)ethan-1-yl]-3H-1,4,8b-triazaacenaphthylen-3-one dihydrochloride

HRID 619499
ノート
印刷プレビュー

反応式

HRID 619499 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][N:16]2[CH2:26][C:25]3[N:27]4[C:18](=[CH:19][N:20]=[C:21]4[CH:22]=[CH:23][CH:24]=3)[C:17]2=[O:28])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:29]>C(O)C>[ClH:29].[ClH:29].[NH:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][N:16]2[CH2:26][C:25]3[N:27]4[C:18](=[CH:19][N:20]=[C:21]4[CH:22]=[CH:23][CH:24]=3)[C:17]2=[O:28])[CH2:10][CH2:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 211902154,5-Dihydro-4-[2-(1-tert-butoxycarbonylpiperidin-4-yl)ethan-1-yl]-3H-1,4,8b-triazaacenaphthylen-3-one

生成物 1

HCID 211901804,5-dihydro-4-[2-(piperidin-4-yl)ethan-1-yl]-3H-1,4,8b-triazaacenaphthylen-3-one dihydrochloride収率 79.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution prepared by dissolving 2.88 g (7.49 mM) of 4,5-dihydro-4-[2-(1-tert-butoxycarbonylpiperidin-4-yl)ethan-1-yl]-3H-1,4,8b-triazaacenaphthylen-3-one in 30 ml of ethanol was added 6.25 ml (74.9 mM) of 12N-hydrochloric acid and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, the reaction mixture was concentrated under reduced pressure and the precipitate was recovered by filtration. The precipitate was rinsed with small amounts of ethanol and ether to provide 2.13 g (yield 79.8%) of the title compound as light-yellow crystals.

後処理

  1. customTo a solution prepared
  2. customAfter completion of the reaction
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. filtrationthe precipitate was recovered by filtration
  5. washThe precipitate was rinsed with small amounts of ethanol and ether

出典と根拠

ORDレコード
ord-ce4fd56062634e45a030a84b4bee15f8
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05958942

反応ノート

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