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Methanol → HCID 67499138, 화합물

HRID 74303
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HRID 74303 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[CH:30]=[CH:29][C:13]2[N:14]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([O:27]C)=[O:26])[CH:20]=3)[C:15]([CH3:17])=[N:16][C:12]=2[CH:11]=1.[OH-].[Na+].CO>C(Cl)(Cl)Cl>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[CH:30]=[CH:29][C:13]2[N:14]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([OH:27])=[O:26])[CH:20]=3)[C:15]([CH3:17])=[N:16][C:12]=2[CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 674984625-(Benzoxazol-2-yl)-1-(3-methoxycarbonylphenylmethyl)-2-methylbenzimidazole

생성물 1

HCID 67499138HCID 67499138, 화합물수율 99.4%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 5-(benzoxazol-2-yl)-1-(3-methoxycarbonylphenylmethyl)-2-methylbenzimidazole (see Working Example 117-2) (125 mg, 0.315 mmol) in chloroform (3 mL) was added aqueous sodium hydroxide solution (1 M, 1 mL, 1 mmol). This two-layer solution was homogenized by the addition of methanol, and this was stirred at room temperature for 20 hours. After the reaction was complete, the solution was concentrated, aqueous acetic acid solution was added, and this was stirred at room temperature. The precipitated crystals were filtered, and after washing with water were dried to yield the title compound (120 mg, 99% yield) as white crystals.

후처리

  1. concentrationthe solution was concentrated
  2. additionaqueous acetic acid solution was added
  3. stirringthis was stirred at room temperature
  4. filtrationThe precipitated crystals were filtered
  5. washafter washing with water
  6. customwere dried

출처 및 근거

ORD 기록
ord-81e80b406c8b43288fdbb6c0ce9fd441
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08829035B2

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