Water → 2-Piperazin-1-yl-benzoic acid sulfuric acid salt

HRID 907577ノート

反応式

HRID 907577 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1)#N.N1CCNCC1.[OH2:21].[OH-:22].[NH4+].[S:24](=[O:28])(=[O:27])([OH:26])[OH:25]>>[S:24](=[O:26])(=[O:25])([OH:28])[OH:27].[N:9]1([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[C:1]([OH:22])=[O:21])[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1

参加物

6

反応物 5

HCID 962WaterHCID 1118Sulfuric AcidHCID 4837PiperazineHCID 14923Ammonium HydroxideHCID 2735875N-(2-Cyanophenyl)piperazine

生成物 1

HCID 673880502-Piperazin-1-yl-benzoic acid sulfuric acid salt

反応条件

温度
100 °C

実験手順

1-(2-Cyanophenyl)piperazine (2.00 g, 10.68 mmol) was suspended in 10 mL of concentrated sulfuric acid. The piperazine slowly dissolved as the reaction mixture was heated to 100° C. After heating the reaction for 2 hr, the reaction was cooled to room temperature. 10 mL of water was added and the reaction was heated to 100° C. for another 4 hr. After cooling to room temperature, the reaction mixture was poured into 200 mL of ice water. The aqueous mixture was neutralized with ammonium hydroxide and the mixture was concentrated under vacuum. The product was extracted from the inorganic salts by washing with 25% methanol in tetrahydrofuran. The crude material was used in the next step without purification.

後処理

  1. temperatureAfter heating
  2. customthe reaction for 2 hr
  3. temperaturethe reaction was cooled to room temperature
  4. temperaturethe reaction was heated to 100° C. for another 4 hr
  5. temperatureAfter cooling to room temperature
  6. concentrationthe mixture was concentrated under vacuum
  7. extractionThe product was extracted from the inorganic salts
  8. washby washing with 25% methanol in tetrahydrofuran
  9. customThe crude material was used in the next step without purification

出典と根拠

ORDレコード
ord-a0c7bb0dc7814a95ab0140e37799f5cd
出典データセット
uspto-grants-2011_09
特許番号
US08013156B2

反応ノート

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