Hydrochloric Acid → HCID 68766365, 화합물

HRID 1628403노트

반응식

HRID 1628403 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:14]([CH2:15][CH2:16][C:17]([O:19]CC)=[O:18])[C:13]2[C:22]([N:26]([CH2:29][CH3:30])[CH2:27][CH3:28])=[CH:23][CH:24]=[CH:25][C:12]=2[N:11]=1.[OH-].[Na+].Cl>O1CCCC1.CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:14]([CH2:15][CH2:16][C:17]([OH:19])=[O:18])[C:13]2[C:22]([N:26]([CH2:27][CH3:28])[CH2:29][CH3:30])=[CH:23][CH:24]=[CH:25][C:12]=2[N:11]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 68761561HCID 68761561, 화합물

생성물 1

HCID 68766365HCID 68766365, 화합물수율 78%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl 3-[2-[(2,4-dichlorophenyl)amino]-7-(diethylamino)-1H-benzimidazol-1-yl]propanoate (Reference Example 28; 100 mg, 0.223 mmol) in a mixture of tetrahydrofuran (2 mL) and methanol (1 mL) was added 1N sodium hydroxide solution (0.446 mL, 0.446 mmol) at 0° C. After the resultant mixture was stirred at room temperature for 1 hr, the mixture was neutralized with 1N hydrochloric acid and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with ethyl acetate to give the title compound as a solid (73.3 mg, 0.174 mmol, 78%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe combined organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatography on silica gel eluting with ethyl acetate

출처 및 근거

ORD 기록
ord-1a0945e85cf34c76a477b95a78ba0b31
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785460B2

반응 노트

불러오는 중…