Sodium Hydroxide → HCID 178492289, 화합물

HRID 638235노트

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HRID 638235 반응식
[OH-].[Na+].[F:3][C:4]1([F:19])[O:17][C:8]2=[CH:9][C:10]3[N:14]=[C:13]([SH:15])[NH:12][C:11]=3[CH:16]=[C:7]2[O:6][CH:5]1[F:18].Cl.Cl[CH2:22][C:23]1[C:28]([CH3:29])=[C:27]([O:30][CH3:31])[C:26]([CH3:32])=[CH:25][N:24]=1>C(O)C>[F:19][C:4]1([F:3])[O:17][C:8]2=[CH:9][C:10]3[N:14]=[C:13]([S:15][CH2:22][C:23]4[C:28]([CH3:29])=[C:27]([O:30][CH3:31])[C:26]([CH3:32])=[CH:25][N:24]=4)[NH:12][C:11]=3[CH:16]=[C:7]2[O:6][CH:5]1[F:18]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 116942582-(Chloromethyl)-3,5-dimethyl-4-methoxypyridine hydrochlorideHCID 178506022HCID 178506022, 화합물

생성물 1

HCID 178492289HCID 178492289, 화합물수율 77%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
40 °C

실험 절차

6.1 ml of 2M sodium hydroxide solution are added dropwise to a mixture of 1.6 g of 6,6,7-trifluoro-6,7-dihydro-1H-[1,4]-dioxino[2,3-f]benzimidazole-2-thiol and 1.4 g of 2-chloromethyl-4-methoxy-3,5-dimethylpyridine hydrochloride in 40 ml of ethanol at room temperature and the mixture is stirred at 40° C. for 5 h. The solvent is distilled off in vacuo, water is added, the mixture is extracted with methylene chloride, the organic solution is concentrated and the residue is recrystallized from ethanol and water. 1.9 g (77%) of the title compound of m.p. 138°-140° C. are obtained.

후처리

  1. distillationThe solvent is distilled off in vacuo, water
  2. additionis added
  3. extractionthe mixture is extracted with methylene chloride
  4. concentrationthe organic solution is concentrated
  5. customthe residue is recrystallized from ethanol and water

출처 및 근거

ORD 기록
ord-70c9a3d34e99416db7d353ede2cbba47
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04560693

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