Hydrochloric Acid → HCID 59309873, 화합물

HRID 1513070노트

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HRID 1513070 반응식
C([O:4][CH:5]([C:7]1[N:15]=[C:14]2[C:10]([NH:11][C:12](=[O:42])[N:13]2[C:16]2[CH:21]=[C:20]([O:22][CH2:23][C:24]3[C:29]([O:30][CH3:31])=[CH:28][CH:27]=[C:26]([F:32])[C:25]=3[F:33])[C:19]([O:34][CH2:35][C:36]([O:38][CH2:39][CH3:40])=[O:37])=[CH:18][C:17]=2[Cl:41])=[C:9]([O:43][CH3:44])[N:8]=1)[CH3:6])(=O)C.C(OC(C1N=C(Cl)C([N+]([O-])=O)=C(OC)N=1)C)(=O)C.NC1C(Cl)=CC(OCC(OCC)=O)=C(OCC2C(OC)=CC=C(F)C=2F)C=1.NC1C(Cl)=CC(OCC(OCC)=O)=C(OCC2C(OC)=CC=CC=2F)C=1.[O-]CC.[Na+].Cl>C(O)C.O1CCCC1>[Cl:41][C:17]1[CH:18]=[C:19]([O:34][CH2:35][C:36]([O:38][CH2:39][CH3:40])=[O:37])[C:20]([O:22][CH2:23][C:24]2[C:29]([O:30][CH3:31])=[CH:28][CH:27]=[C:26]([F:32])[C:25]=2[F:33])=[CH:21][C:16]=1[N:13]1[C:12](=[O:42])[NH:11][C:10]2[C:14]1=[N:15][C:7]([CH:5]([OH:4])[CH3:6])=[N:8][C:9]=2[O:43][CH3:44]

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 59309820HCID 59309820, 화합물HCID 59309837HCID 59309837, 화합물HCID 59309965HCID 59309965, 화합물HCID 68511706HCID 68511706, 화합물

생성물 1

HCID 59309873HCID 59309873, 화합물수율 55.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2-(1-acetyloxyethyl)-9-[2-chloro-4-ethoxycarbonylmethoxy-5-(2,3-difluoro-6-methoxybenzyloxy)phenyl]-6-methoxy-7,9-dihydro-8H-purin-8-one (0.33 g), which was prepared in a similar manner to that described in Example 171 using 2-(1-acetyloxyethyl)-4-chloro-6-methoxy-5-nitropyrimidine and ethyl 2-[4-amino-5-chloro-2-(2,3-difluoro-6-methoxybenzyloxy)phenoxy]acetate instead of 4-chloro-6-methoxy-2-methoxymethyl-5-nitropyrimidine and ethyl 2-[4-amino-5-chloro-2-(2-fluoro-6-methoxy-benzyloxy)phenoxy]acetate, respectively, in ethanol (2 mL)-tetrahydrofuran (3 mL) was added sodium ethoxide (20% ethanol solution, 0.5 mL), and the mixture was stirred at room temperature for 3 hours. The reaction mixture was poured into 1 mol/L hydrochloric acid, and the resulting mixture was extracted with ethyl acetate. The extract was washed with water and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=1/1−1/9) to give the title compound (0.17 g)

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe extract was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=1/1−1/9)

출처 및 근거

ORD 기록
ord-f833b9fe5e774c5bb5c63e9180f3b3b3
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217069B2

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