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

HRID 868716

반응식

HRID 868716 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cafdf8457e794dab9ea640a7878cba54
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04780561

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