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Diisopropyl Ether → 6-(4-Oxo-4H-1,3-benzothiazin-2-yl)-2-pyridinecarboxylic acid

HRID 748156
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반응식

HRID 748156 반응식
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5][C:4]([C:12]2[N:17]=[C:16]([C:18]([O:20]C(C)(C)C)=[O:19])[CH:15]=[CH:14][CH:13]=2)=[N:3]1.C(OC(C)C)(C)C>FC(F)(F)C(O)=O>[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5][C:4]([C:12]2[N:17]=[C:16]([C:18]([OH:20])=[O:19])[CH:15]=[CH:14][CH:13]=2)=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7914Diisopropyl EtherHCID 22939348tert-Butyl 6-(4-oxo-4H-1,3-benzothiazin-2-yl)-2-pyridinecarboxylate

생성물 1

HCID 229393396-(4-Oxo-4H-1,3-benzothiazin-2-yl)-2-pyridinecarboxylic acid수율 78.3%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A mixture of tert-butyl 6-(4-oxo-4H-1,3-benzothiazin-2-yl)-2-pyridinecarboxylate (400 mg, 1.1 mmol) and trifluoroacetic acid (10 ml) was stirred under ice cooling condition for 3 hrs. The reaction mixture was combined with diisopropylether to precipitate crystals, which were collected by filtration and recrystallized from methanol-diisopropylether to give the titled compound (245 mg, 73%).

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후처리

  1. customto precipitate crystals, which
  2. filtrationwere collected by filtration
  3. customrecrystallized from methanol-diisopropylether

출처 및 근거

ORD 기록
ord-81ffcc65dc4f4e9a9ca5bcafcc092b2e
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07399759B2

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