Lithium Hydroxide → HCID 24959696, 화합물

HRID 2381853노트

반응식

HRID 2381853 반응식
[CH3:1][C:2]1[CH:6]=[C:5]([N:7]2[N:11]=[N:10][C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[N:8]2)[S:4][C:3]=1[C:18]([O:20]CC)=[O:19].O1CCCC1.[OH-].[Li+]>O>[CH3:1][C:2]1[CH:6]=[C:5]([N:7]2[N:11]=[N:10][C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[N:8]2)[S:4][C:3]=1[C:18]([OH:20])=[O:19]

참가 물질

5

반응물 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 24959335HCID 24959335, 화합물

생성물 1

HCID 24959696HCID 24959696, 화합물수율 82.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of ethyl 3-methyl-5-(5-phenyl-2H-tetrazol-2-yl)thiophene-2-carboxylate (0.16 g, 0.51 mmol) in a 1:1 mixture of tetrahydrofuran:water (10 mL) was added lithium hydroxide (0.11 g, 2.55 mmol). The reaction mixture was refluxed for 18 hours and allowed to cool to ambient temperature. The organic solvent was removed in vacuo. The aqueous solution was acidified with 10% aqueous solution. The white solid was collected by filtration, washed with water and dried to afford the title compound as red colored solid (0.12 g, 82%): 1H NMR (300 MHz, DMSO-d6) δ 8.14-8.11 (m, 2H), 7.75 (s, 1H), 7.62-7.60 (m, 3H), 2.54 (s, 3H); MS (ES+) m/z 287.2 (M+1).

후처리

  1. temperatureThe reaction mixture was refluxed for 18 hours
  2. customThe organic solvent was removed in vacuo
  3. filtrationThe white solid was collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-b687c5d01b56436ea56ff8b1219cb8a3
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258160B2

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