Hydrochloric Acid → 5-(Benzoxazol-2-yl)-2-methyl-1-(2-carboxy-n-propyl)benzimidazole

HRID 74304노트

반응식

HRID 74304 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:29]=[CH:28][C:13]2[N:14]([CH2:18][CH:19]([C:21]([O:23]C(C)(C)C)=[O:22])[CH3:20])[C:15]([CH3:17])=[N:16][C:12]=2[CH:11]=1.[OH-].[Li+].Cl>C1COCC1.O>[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:29]=[CH:28][C:13]2[N:14]([CH2:18][CH:19]([C:21]([OH:23])=[O:22])[CH3:20])[C:15]([CH3:17])=[N:16][C:12]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 674984575-(Benzoxazol-2-yl)-2-methyl-1-(2-tert-butoxycarbonyl-n-propyl)benzimidazole

생성물 1

HCID 680688295-(Benzoxazol-2-yl)-2-methyl-1-(2-carboxy-n-propyl)benzimidazole수율 86.5%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

5-(Benzoxazol-2-yl)-2-methyl-1-(2-tert-butoxycarbonyl-n-propyl)benzimidazole (see Working Example 121-2) (0.4 g, 1.0 mmol) and THF/water=2:1 (40 mL) were charged, and lithium hydroxide (0.043 g, 1.0 mmol) was added at room temperature, and this was heated and stirred for 5 hours. After being kept cool, the liquid was brought to approximately pH 5 with dilute hydrochloric acid (1 M), the crystals obtained were filtered off and washed with distilled water, and then were dried with heating under reduced pressure to yield the title compound (0.29 g, 83% yield) as white crystals.

후처리

  1. temperaturethis was heated
  2. temperatureAfter being kept cool
  3. customthe crystals obtained
  4. filtrationwere filtered off
  5. washwashed with distilled water
  6. customwere dried
  7. temperaturewith heating under reduced pressure

출처 및 근거

ORD 기록
ord-f25faacc7fe94f34b39ff0e1f3edce43
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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