Sodium hydride → HCID 131730788, 화합물

HRID 80944

반응식

HRID 80944 반응식
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:15]=[N:14][C:13]([C:16]3[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=3)=[CH:12][CH:11]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[H-].[Na+].[Cl:25][CH2:26][C:27]([N:29]([CH3:31])[CH3:30])=[O:28]>CN(C=O)C>[ClH:25].[ClH:25].[CH:1]([N:4]1[CH2:5][CH2:6][N:7]([C:10]2[N:15]=[N:14][C:13]([C:16]3[CH:17]=[CH:18][C:19]([O:22][CH2:26][C:27]([N:29]([CH3:31])[CH3:30])=[O:28])=[CH:20][CH:21]=3)=[CH:12][CH:11]=2)[CH2:8][CH2:9]1)([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 758862-chloro-N,N-dimethylacetamideHCID 1360994094-(6-(4-Isopropylpiperazin-1-yl)-pyridazin-3-yl)-phenol

생성물 1

HCID 131730788HCID 131730788, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A mixture of 4-[6-(4-isopropyl-piperazin-1-yl)-pyridazin-3-yl]-phenol (110 mg, 0.37 mmol) and 60% sodium hydride (58 mg, 1.45 mmol) in dry DMF (5 mL) was heated at 60° C. for 30 min. 2-Chloro-N,N-dimethylacetamide (54 mg, 0.44 mmol) was added and heating at 60° C. was continued for another 20 h. The reaction mixture was evaporated to dryness and partitioned between water (10 mL) and DCM (10 mL). The organic phase was isolated, washed with brine (5 mL), dried over anhydrous magnesium sulphate, and evaporated to dryness in vacuo. The residue was dissolved in hot ethyl acetate and HClg in Et2O was added to give the title compound.

후처리

  1. temperatureheating at 60° C.
  2. customThe reaction mixture was evaporated to dryness
  3. custompartitioned between water (10 mL) and DCM (10 mL)
  4. customThe organic phase was isolated
  5. washwashed with brine (5 mL)
  6. dry with materialdried over anhydrous magnesium sulphate
  7. customevaporated to dryness in vacuo
  8. dissolutionThe residue was dissolved in hot ethyl acetate
  9. additionHClg in Et2O was added

출처 및 근거

ORD 기록
ord-ad58286448e340c4add39b118395f36f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846677B2

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