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Tetrahydrofuran → [4-(3,5-Dimethylpyridin-2-yl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-2-methylphenyl]methanone hydrobromide

HRID 2411581
ノート
印刷プレビュー

反応式

HRID 2411581 の反応式
[CH3:1][C:2]1[C:3]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([C:17]3[CH:22]=[CH:21][C:20]([N:23]4[CH2:27][CH2:26][CH2:25][S:24]4(=[O:29])=[O:28])=[CH:19][C:18]=3[CH3:30])=[O:16])[CH2:11][CH2:10]2)=[N:4][CH:5]=[C:6]([CH3:8])[CH:7]=1.[BrH:31].C(O)(=O)C.O1CCCC1>C(O)(=O)C>[BrH:31].[CH3:1][C:2]1[C:3]([N:9]2[CH2:10][CH2:11][N:12]([C:15]([C:17]3[CH:22]=[CH:21][C:20]([N:23]4[CH2:27][CH2:26][CH2:25][S:24]4(=[O:29])=[O:28])=[CH:19][C:18]=3[CH3:30])=[O:16])[CH2:13][CH2:14]2)=[N:4][CH:5]=[C:6]([CH3:8])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 21893785Acetic Acid Mixture with Hydrobromic AcidHCID 71252659[4-(3,5-Dimethylpyridin-2-yl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-2-methylphenyl]methanone

生成物 1

HCID 86676782[4-(3,5-Dimethylpyridin-2-yl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-2-methylphenyl]methanone hydrobromide

試薬・触媒・溶媒 1

HCID 176
Acetic Acid
溶媒

実験手順

[4-(3,5-Dimethylpyridin-2-yl)piperazin-1-yl][4-(1,1-dioxo-1λ6-isothiazolidin-2-yl)-2-methylphenyl]methanone (5.00 g) described in Example 154 was dissolved in acetic acid (20 mL), and 25% hydrogen bromide/acetic acid (3.3 mL) was added at 50° C. The reaction mixture was allowed to cool to room temperature, tetrahydrofuran (200 mL) was added, and the precipitate was collected by filtration. The obtained precipitate (5.52 g) was recrystallized from ethanol (110 mL) to give the title compound (4.67 g).

後処理

  1. filtrationthe precipitate was collected by filtration
  2. customThe obtained precipitate (5.52 g) was recrystallized from ethanol (110 mL)

出典と根拠

ORDレコード
ord-a886670ccd334cfd9165706df49c0692
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08816079B2

反応ノート

読み込み中…

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