Hydrochloric Acid → HCID 58012318, 화합물

HRID 1398741노트

반응식

HRID 1398741 반응식
[Cl:1][C:2]1[C:10]2[N:9]=[C:8]([NH:11][C:12]3[C:17]([CH3:18])=[CH:16][C:15]([Cl:19])=[CH:14][C:13]=3[O:20][CH3:21])[N:7]([CH2:22][C:23]([O:25]C(C)C)=[O:24])[C:6]=2[C:5]([CH:29]([CH2:32][CH3:33])[CH2:30][CH3:31])=[CH:4][CH:3]=1.[OH-].[Na+].O.Cl>CO>[Cl:1][C:2]1[C:10]2[N:9]=[C:8]([NH:11][C:12]3[C:17]([CH3:18])=[CH:16][C:15]([Cl:19])=[CH:14][C:13]=3[O:20][CH3:21])[N:7]([CH2:22][C:23]([OH:25])=[O:24])[C:6]=2[C:5]([CH:29]([CH2:32][CH3:33])[CH2:30][CH3:31])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 58012354HCID 58012354, 화합물

생성물 1

HCID 58012318HCID 58012318, 화합물수율 99.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of isopropyl [4-chloro-2-[(4-chloro-2-methoxy-6-methylphenyl)amino]-7-(1-ethylpropyl)-1H-benzimidazol-1-yl]acetate (Reference Example 11; 861 mg, 1.75 mmol) in methanol (5 mL) was added 8N aqueous sodium hydroxide (1.5 mL), and the mixture was stirred at room temperature for 15 hr. Water was added to the reaction mixture, followed by neutralization with 6N hydrochloric acid. The mixture was concentrated in vacuo, and the residue was dissolved in methanol. The precipitate was removed by filtration, and the filtrate was concentrated in vacuo to give the title compound (781 mg, 1.73 mmol, 99.1%) as an amorphous.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in methanol
  3. customThe precipitate was removed by filtration
  4. concentrationthe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-94c99044ac2d4581900c98057e93562d
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901141B2

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