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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
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인쇄 미리보기

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HRID 2411581 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 176
Acetic Acid
용매

실험 절차

[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).

후처리

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

출처 및 근거

ORD 기록
ord-a886670ccd334cfd9165706df49c0692
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08816079B2

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