Sodium Hydroxide → HCID 67333043、化合物

HRID 1672253ノート

反応式

HRID 1672253 の反応式
C[O:2][C:3](=[O:24])[CH2:4][CH2:5][CH:6]([NH:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:14][CH:13]=1)=[O:11])[CH2:7][OH:8].[OH-].[Na+]>C1COCC1.CO>[C:15]1([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:14]=[CH:13][C:12]([C:10]([NH:9][CH:6]([CH2:7][OH:8])[CH2:5][CH2:4][C:3]([OH:24])=[O:2])=[O:11])=[CH:17][CH:16]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 67332127HCID 67332127、化合物

生成物 1

HCID 67333043HCID 67333043、化合物収率 76.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 4-[(Biphenyl-4-carbonyl)-amino]-5-hydroxy-pentanoic acid methyl ester (333 mg, 1.06 mmol) in THF (10 mL) and MeOH (1.27 mL) was added to 1N NaOH (1.27 mL, 1.27 mmol, 1.2 equiv) at room temperature. The mixture was stirred for 2 hours and TLC indicated the reaction was complete. Solvent was removed and the residue was dissolved in water. After adjusting the pH to 4 with 1N HCl, solid precipitated from the solution. The solid was then collected by filtration, washed with water, and dried under vacuum overnight to afford 240 mg of 4-[(Biphenyl-4-carbonyl)-amino]-5-hydroxy-pentanoic acid in 76.7% yield. MS (ESI) m/z 314.

後処理

  1. customSolvent was removed
  2. dissolutionthe residue was dissolved in water
  3. customprecipitated from the solution
  4. filtrationThe solid was then collected by filtration
  5. washwashed with water
  6. customdried under vacuum overnight

出典と根拠

ORDレコード
ord-93c76c5813e94c0b892d92083c709f73
出典データセット
uspto-grants-2011_08
特許番号
US07998965B2

反応ノート

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