Sodium Hydroxide → 1-(4-Formylbenzoyl)-4-isopropylpiperazine

HRID 13546

반응식

HRID 13546 반응식
[Na+].[OH:2][CH:3]([C:8]1[CH:13]=[CH:12][C:11]([C:14]([N:16]2[CH2:21][CH2:20][N:19]([CH:22]([CH3:24])[CH3:23])[CH2:18][CH2:17]2)=[O:15])=[CH:10][CH:9]=1)S([O-])(=O)=O.[OH-].[Na+]>O>[CH:22]([N:19]1[CH2:20][CH2:21][N:16]([C:14]([C:11]2[CH:10]=[CH:9][C:8]([CH:3]=[O:2])=[CH:13][CH:12]=2)=[O:15])[CH2:17][CH2:18]1)([CH3:24])[CH3:23]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 59340029Hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl)-phenyl]-methanesulfonic acid sodium salt

생성물 1

HCID 574785811-(4-Formylbenzoyl)-4-isopropylpiperazine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

To a suspension of hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl) -phenyl]-methanesulfonic acid sodium salt (49.0 g, 135 mmol) in de-ionized H2O (490 mL) at 0° C. was added 1 N NaOH (100 mL) in 10 mL portions with vigorous stirring. A clear solution resulted (pH 12), which was stirred at 0° C. for 1 h, then at room temperature for 30 min. The aqueous solution was extracted with EtOAc (3×200 mL), followed by CH2Cl2 (3×200 mL). The organic layers were combined, washed with brine (1×300 mL), dried (Na2SO4) and concentrated to yield the title compound as a pale yellow oil.

후처리

  1. customA clear solution resulted (pH 12), which
  2. waitat room temperature for 30 min
  3. extractionThe aqueous solution was extracted with EtOAc (3×200 mL)
  4. washwashed with brine (1×300 mL)
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0b1125e676684ac0b06b4919e8d322df
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728129B2

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