Hydrochloric Acid → HCID 59309873、化合物

HRID 1513070ノート

反応式

HRID 1513070 の反応式
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]

参加物

9

反応物 6

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 59309820HCID 59309820、化合物HCID 59309837HCID 59309837、化合物HCID 59309965HCID 59309965、化合物HCID 68511706HCID 68511706、化合物

生成物 1

HCID 59309873HCID 59309873、化合物収率 55.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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)

後処理

  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)

出典と根拠

ORDレコード
ord-f833b9fe5e774c5bb5c63e9180f3b3b3
出典データセット
uspto-grants-2012_07
特許番号
US08217069B2

反応ノート

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