Lithium Hydroxide → Benzoic Acid

HRID 507399ノート

反応式

HRID 507399 の反応式
C([O:3][C:4](=[O:33])[C:5]1[CH:10]=[CH:9][C:8](C(=O)CN2C(=O)C(C3C=CC=CC=3)(C3C=CC=CC=3)N=C2C)=[CH:7][CH:6]=1)C.[Li+].[OH-]>O1CCOCC1>[C:4]([OH:33])(=[O:3])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 684640534-[2-(2-Methyl-5-oxo-4,4-diphenyl4,5-dihydro-imidazol-1-yl)-acetyl]-benzoic acid ethyl ester

生成物 1

HCID 243Benzoic Acid収率 296.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

4-[2-(2-Methyl-5-oxo-4,4-diphenyl4,5-dihydro-imidazol-1-yl)-acetyl]-benzoic acid ethyl ester (540 mg, 1.2 mmol) is dissolved in 12 mL dioxane and an aqueous 2 Molar LiOH solution (920 uL, 1.8 mmol) is added drop wise. The reaction mixture is stirred at room temperature for 12 hours. Subsequently the mixture is evaporated and the residue taken up in water. The mixture is stirred and concentrated hydrochloric acid is added drop wise until a pH of 2 is reached. The precipitating crystals are filtered off, re-crystallized from methylene chloride and dried to yield 4-[2-2-methyl-5-oxo-4,4-diphenyl-4,5-dihydro-imidazol-1-yl)-acetyl]-benzoic acid (435 mg, 84%) light yellow solid. LC/MS at 254 nm; [M+H] 413; Rt 3.154 min.

後処理

  1. customSubsequently the mixture is evaporated
  2. stirringThe mixture is stirred
  3. additionconcentrated hydrochloric acid is added drop wise until a pH of 2
  4. filtrationThe precipitating crystals are filtered off
  5. customre-crystallized from methylene chloride
  6. customdried

出典と根拠

ORDレコード
ord-3b7c70f0fc014a7eb335052a75056187
出典データセット
uspto-grants-2010_08
特許番号
US07786155B2

反応ノート

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