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Lithium hydroxide, monohydrate → HCID 24826505, 화합물

HRID 910971
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HRID 910971 반응식
[CH3:1][C:2]1[N:3]=[C:4]([NH:7][C:8]2[CH:18]=[C:17]([O:19][C:20]3[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:23]=[CH:22][CH:21]=3)[C:11]([C:12]([O:14]CC)=[O:13])=[CH:10][N:9]=2)[S:5][CH:6]=1.O.[OH-].[Li+]>C1COCC1.O>[CH3:1][C:2]1[N:3]=[C:4]([NH:7][C:8]2[CH:18]=[C:17]([O:19][C:20]3[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:23]=[CH:22][CH:21]=3)[C:11]([C:12]([OH:14])=[O:13])=[CH:10][N:9]=2)[S:5][CH:6]=1
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 24825976HCID 24825976, 화합물

생성물 1

HCID 24826505HCID 24826505, 화합물수율 65.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 6-(4-methylthiazol-2-ylamino)-4-(naphthalen-1-yloxy)nicotinate (1.00 g, 2.47 mmol) was dissolved in THF (5 mL). A solution of lithium hydroxide hydrate (0.207 g, 4.93 mmol) in water (1 mL) was added, and the reaction mixture was stirred at room temperature overnight. The reaction mixture was concentrated, 2M HCl was added to adjust the pH to 3. The reaction mixture was filtered to obtain the desired product (0.61 g, 65.5% yield) as a white solid. 1H NMR (d6-DMSO) δ 10.85 (bs, 1H), 8.76 (s, 1H), 8.06 (d, 1H), 7.88-7.93 (m, 2H), 7.55-7.65 (m, 3H), 7.35 (d, 1H), 6.58 (s, 1H), 6.32 (s, 1H), 2.14 (s, 3H).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. addition2M HCl was added
  3. filtrationThe reaction mixture was filtered

출처 및 근거

ORD 기록
ord-1bd7fd5fba2f4b3ba09d41526eae20f1
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022222B2

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