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

HRID 5522ノート

反応式

HRID 5522 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 1-methyl-4-(3,4-diacetoxybenzoyl)piperazine (295 mg) n methanol (3 ml) was added a saturated potassium carbonate solution is 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.

後処理

  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

出典と根拠

ORDレコード
ord-a8eca58fbacb432c81e4d18ca5413a11
出典データセット
uspto-grants-1993_09
特許番号
US05244890

反応ノート

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