Hydrochloric Acid → HCID 49806002、化合物

HRID 1615060ノート

反応式

HRID 1615060 の反応式
[CH:1]1([C:4]2[CH:48]=[CH:47][C:7]([CH2:8][O:9][C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:19][N:18]([C:20]([C:22]5[CH:27]=[C:26]([CH2:28][O:29][CH2:30][C:31]6([CH2:43][OH:44])[CH2:36][O:35]C(C7C=CC=CC=7)[O:33][CH2:32]6)[CH:25]=[CH:24][N:23]=5)=[O:21])[CH2:17]4)=[CH:12][C:11]=3[O:45][CH3:46])=[CH:6][CH:5]=2)[CH2:3][CH2:2]1.Cl.[OH-].[Na+].C([O-])(O)=O.[Na+]>O1CCCC1>[CH:1]1([C:4]2[CH:48]=[CH:47][C:7]([CH2:8][O:9][C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:17][N:18]([C:20]([C:22]5[CH:27]=[C:26]([CH2:28][O:29][CH2:30][C:31]([CH2:32][OH:33])([CH2:36][OH:35])[CH2:43][OH:44])[CH:25]=[CH:24][N:23]=5)=[O:21])[CH2:19]4)=[CH:12][C:11]=3[O:45][CH3:46])=[CH:6][CH:5]=2)[CH2:2][CH2:3]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 59634057HCID 59634057、化合物2 回

生成物 1

HCID 49806002HCID 49806002、化合物収率 44%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of the crude {3-[4-(4-cyclopropylbenzyloxy)-3-methoxyphenyl]azetidin-1-yl}-[4-(5-hydroxymethyl-2-phenyl-[1,3]dioxan-5-ylmethoxymethyl)-pyridin-2-yl]-methanone prepared in (1) in THF (10 mL) was added 1 N hydrochloric acid (5.0 mL). The reaction mixture was stirred at RT for 24 hr. To the reaction mixture were added aqueous 1 N NaOH and saturated aqueous NaHCO3 and then the mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by silica gel chromatography (Developing solvent: chloroform/methanol=5/1) to give the title compound (0.33 g, 44%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over MgSO4
  3. customThe solvent was removed under reduced pressure
  4. customThe residue was purified by silica gel chromatography (Developing solvent: chloroform/methanol=5/1)

出典と根拠

ORDレコード
ord-c5d4214a80404bf897b515c0be28a41c
出典データセット
uspto-grants-2014_07
特許番号
US08765739B2

反応ノート

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