Sodium Hydroxide → 4-(2-Oxo-2,3-dihydro-1H-benzimidazol-1-yl)butanoic acid

HRID 1381098노트

반응식

HRID 1381098 반응식
[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][CH2:9][C:10]([O:12]CC)=[O:11])[C:5]2[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=2[NH:3]1.[OH-].[Na+]>CO>[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])[C:5]2[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=2[NH:3]1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 103997611H-Benzimidazole-1-butanoic acid, 2,3-dihydro-2-oxo-, ethyl ester

생성물 1

HCID 132517844-(2-Oxo-2,3-dihydro-1H-benzimidazol-1-yl)butanoic acid수율 92.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 22 g of the product of Step B, 22 ml of sodium hydroxide solution and 200 ml of methanol was refluxed for one hour and the methanol was evaporated. The residue was taken up in 1.5 liters of iced water and the pH was adjusted to 1 by addition of concentrated hydrochloric acid. The mixture was vacuum filtered and the product was washed with water to obtain 18.1 g of 2,3-dihydro-2-oxo-1H-benzimidazol-1-butanoic acid melting at 180° C. The product was crystallized from isopropanol to obtain 15.2 g of product melting at 185° C.

후처리

  1. customthe methanol was evaporated
  2. additionthe pH was adjusted to 1 by addition of concentrated hydrochloric acid
  3. filtrationfiltered
  4. washthe product was washed with water

출처 및 근거

ORD 기록
ord-94f44e8a2dd0406187b2a315f4518f5e
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04585770

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