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Hydrochloric Acid → HCID 67463201, 화합물

HRID 1619951
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HRID 1619951 반응식
[CH2:1]([CH:3]1[C:8]([C:9]2[CH:24]=[CH:23][C:12]3[N:13]=[C:14]([C:16]4[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=4)[O:15][C:11]=3[CH:10]=2)=[N:7][NH:6][C:5](=[O:25])[CH2:4]1)[CH3:2].Cl[CH2:27][CH:28]([N:30]1[CH2:34][CH2:33][CH2:32][CH2:31]1)[CH3:29].Cl.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:1]([CH:3]1[C:8]([C:9]2[CH:24]=[CH:23][C:12]3[N:13]=[C:14]([C:16]4[CH:21]=[CH:20][C:19]([O:22][CH2:27][CH:28]([N:30]5[CH2:34][CH2:33][CH2:32][CH2:31]5)[CH3:29])=[CH:18][CH:17]=4)[O:15][C:11]=3[CH:10]=2)=[N:7][NH:6][C:5](=[O:25])[CH2:4]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 122132361-(1-Chloropropan-2-yl)pyrrolidineHCID 1360889275-ethyl-6-[2-(4-hydroxy-phenyl)-benzoxazol-6-yl]-4,5-dihydro-2H-pyridazin-3-one

생성물 1

HCID 67463201HCID 67463201, 화합물

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

40 mg (119 μmol) 5-ethyl-6-[2-(4-hydroxy-phenyl)-benzoxazol-6-yl]-4,5-dihydro-2H-pyridazin-3-one, 23.5 mg (128 μmol) 1-(2-chloro-1-methylethyl)pyrrolidine×HCl, 50 mg (362 μmol) potassium carbonate and 2 ml DMF are heated together for 6 h to 80° C. Then the mixture is extracted with 10% sodium carbonate solution and EA. The org. phase is washed with sat. saline solution, dried on sodium sulphate and then the solv. is totally eliminated i.V. The residue is separated by semipreparative HPLC-MS. (xBridge, MeOH/H2O+TFA)

후처리

  1. extractionThen the mixture is extracted with 10% sodium carbonate solution and EA
  2. washphase is washed with sat. saline solution
  3. customdried on sodium sulphate
  4. customThe residue is separated by semipreparative HPLC-MS

출처 및 근거

ORD 기록
ord-6fdda7cbdd5443b9b01588bd72605128
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772323B2

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