Hydrochloric Acid → 3-Carboxymethyl-6-benzyl-2,5-diketopiperazine

HRID 868716ノート

反応式

HRID 868716 の反応式
C[O:2][C:3](=[O:20])[CH2:4][CH:5]1[C:10](=[O:11])[NH:9][CH:8]([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:7](=[O:19])[NH:6]1.[OH-].[Na+].Cl>CO>[CH2:12]([CH:8]1[C:7](=[O:19])[NH:6][CH:5]([CH2:4][C:3]([OH:20])=[O:2])[C:10](=[O:11])[NH:9]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 138837735-Benzyl-3,6-dioxo-2-piperazine acetic acid methyl ester

生成物 1

HCID 1194943-Carboxymethyl-6-benzyl-2,5-diketopiperazine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 1,000 l of a 50% aqueous methanol solution was suspended 55 g of the 5-benzyl-3,6-dioxo-2-piperazine acetic acid methyl ester obtained in Example 1, and 42 g of a 20% aqueous sodium hydroxide solution was added to the suspension at room temperature under stirring. Then, the hydrolysis was conducted at room temperature for two hours to form an aqueous solution. Thereafter, conc. hydrochloric acid was added dropwise to the aqueous solution, which had been removed with methanol under reduced pressure by distillation, to adjust its pH at 1. The resulting mixture was stirred at room temperature for one hour and the crystal thereby deposited was filtered, washed with water and dried to obtain 5-benzyl-3,6-dioxo-2-piperazine acetic acid.

後処理

  1. additionwas added to the suspension at room temperature
  2. customto form an aqueous solution
  3. customhad been removed with methanol under reduced pressure by distillation
  4. stirringThe resulting mixture was stirred at room temperature for one hour
  5. filtrationthe crystal thereby deposited was filtered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-cafdf8457e794dab9ea640a7878cba54
出典データセット
uspto-grants-1988_10
特許番号
US04780561

反応ノート

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