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

HRID 74304ノート

反応式

HRID 74304 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f25faacc7fe94f34b39ff0e1f3edce43
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

反応ノート

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