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Hydrochloric Acid → 6-[4-[2-[(tert-butoxycarbonyl)[(2R)-2-(3-chlorophenyl)-2-hydroxyethyl]amino]ethyl]phenyl]-2-naphthoic acid

HRID 2078662
ノート
印刷プレビュー

反応式

HRID 2078662 の反応式
[C:1]([O:5][C:6]([N:8]([CH2:31][C@@H:32]([C:34]1[CH:39]=[CH:38][CH:37]=[C:36]([Cl:40])[CH:35]=1)[OH:33])[CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:18]=[C:19]3[C:24](=[CH:25][CH:26]=2)[CH:23]=[C:22]([C:27]([O:29]C)=[O:28])[CH:21]=[CH:20]3)=[CH:13][CH:12]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].Cl.C(Cl)(Cl)Cl.CO>O1CCOCC1>[C:1]([O:5][C:6]([N:8]([CH2:31][C@@H:32]([C:34]1[CH:39]=[CH:38][CH:37]=[C:36]([Cl:40])[CH:35]=1)[OH:33])[CH2:9][CH2:10][C:11]1[CH:12]=[CH:13][C:14]([C:17]2[CH:18]=[C:19]3[C:24](=[CH:25][CH:26]=2)[CH:23]=[C:22]([C:27]([OH:29])=[O:28])[CH:21]=[CH:20]3)=[CH:15][CH:16]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21584188Chloroform methanolHCID 67097731methyl 6-[4-[2-[(tert-butoxycarbonyl)[(2R)-2-(3-chlorophenyl)-2-hydroxyethyl]amino]ethyl]phenyl]-2-naphthoate

生成物 1

HCID 670970246-[4-[2-[(tert-butoxycarbonyl)[(2R)-2-(3-chlorophenyl)-2-hydroxyethyl]amino]ethyl]phenyl]-2-naphthoic acid収率 97.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of methyl 6-[4-[2-[(tert-butoxycarbonyl)-[(2R)-2-(3-chlorophenyl)-2-hydroxyethyl]amino]ethyl]-phenyl]-2-naphthoate (105 mg) and 1N sodium hydroxide (0.375 ml) in 1,4-dioxane (1 ml) was stirred at room temperature for 12 hours. To the resulting mixture were added 1N hydrochloric acid (0.375 ml) and chloroform-methanol (5:1). After separation, the organic layer was dried over anhydrous magnesium sulfate, evaporated under reduced pressure. The residue was purified by column chromatography on silica gel (chlorofom/methanol=10/1) to give 6-[4-[2-[(tert-butoxycarbonyl)[(2R)-2-(3-chlorophenyl)-2-hydroxyethyl]amino]ethyl]phenyl]-2-naphthoic acid (100 mg).

後処理

  1. customAfter separation
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. customevaporated under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel (chlorofom/methanol=10/1)

出典と根拠

ORDレコード
ord-b5cf39df9d0a4c0c91cab9945d9cf355
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928264B2

反応ノート

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