Hydrochloric Acid → Piperazine, 1-(3,4-dihydroxybenzoyl)-4-methyl-

HRID 1734266노트

반응식

HRID 1734266 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8](=[O:23])[C:9]2[CH:14]=[CH:13][C:12]([O:15]C(=O)C)=[C:11]([O:19]C(=O)C)[CH:10]=2)[CH2:4][CH2:3]1.C(=O)([O-])[O-].[K+].[K+].Cl>CO>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8](=[O:23])[C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[C:11]([OH:19])[CH:10]=2)[CH2:4][CH2:3]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 150773061-Methyl-4-(3,4-diacetoxybenzoyl)piperazine

생성물 1

HCID 3062451Piperazine, 1-(3,4-dihydroxybenzoyl)-4-methyl-수율 32.6%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of 1-methyl-4-(3,4-diacetoxybenzoyl)piperazine (295 mg) in methanol (3 ml) was added a saturated potassium carbonate solution in methanol (6 ml) and the mixture was stirred at room temperature for 30 minutes. The mixture was poured into ice water and adjusted to pH 9 with 1N hydrochloric acid. The mixture was extracted several times with a mixture of chloroform and methanol (20:1 V/V) and the organic layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was crystallized by addition of ethyl acetate to give 1-methyl-4-(3,4-dihydroxybenzoyl)piperazine (71 mg) as white crystal.

후처리

  1. extractionThe mixture was extracted several times
  2. additionwith a mixture of chloroform and methanol (20:1 V/V)
  3. washthe organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was crystallized by addition of ethyl acetate

출처 및 근거

ORD 기록
ord-91322c5ef7ca450f8623e54b39d6d5f7
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532354

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