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Hydrochloric Acid → N-methyl-N-(2,3,4,5,6-pentahydroxyhexyl)-6-(4-{1-(4-fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-2-yl}phenyl)hex-5-enamide

HRID 2104930
ノート
印刷プレビュー

反応式

HRID 2104930 の反応式
[CH3:1][N:2]([CH2:46][CH:47]([OH:56])[CH:48]([OH:55])[CH:49]([OH:54])[CH:50]([OH:53])[CH2:51][OH:52])[C:3](=[O:45])[CH2:4][CH2:5][CH2:6][CH:7]=[CH:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]2[CH:18]([CH2:19][CH2:20][CH:21]([O:29][Si](C(C)(C)C)(C)C)[C:22]3[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=3)[C:17](=[O:37])[N:16]2[C:38]2[CH:43]=[CH:42][C:41]([F:44])=[CH:40][CH:39]=2)=[CH:11][CH:10]=1.Cl.[OH-].[Na+]>CO>[CH3:1][N:2]([CH2:46][CH:47]([OH:56])[CH:48]([OH:55])[CH:49]([OH:54])[CH:50]([OH:53])[CH2:51][OH:52])[C:3](=[O:45])[CH2:4][CH2:5][CH2:6][CH:7]=[CH:8][C:9]1[CH:10]=[CH:11][C:12]([CH:15]2[CH:18]([CH2:19][CH2:20][CH:21]([C:22]3[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=3)[OH:29])[C:17](=[O:37])[N:16]2[C:38]2[CH:39]=[CH:40][C:41]([F:44])=[CH:42][CH:43]=2)=[CH:13][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 68552127N-methyl-N-(2,3,4,5,6-pentahydroxyhexyl)-6-{4-[3-[3-(tert-butyldimethylsilanyloxy)-3-(4-fluorophenyl)propyl]-1-(4-fluorophenyl)-4-oxoazetidin-2-yl]phenyl}hex-5-enamide

生成物 1

HCID 68551149N-methyl-N-(2,3,4,5,6-pentahydroxyhexyl)-6-(4-{1-(4-fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-2-yl}phenyl)hex-5-enamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

70 mg of N-methyl-N-(2,3,4,5,6-pentahydroxyhexyl)-6-{4-[3-[3-(tert-butyldimethylsilanyloxy)-3-(4-fluorophenyl)propyl]-1-(4-fluorophenyl)-4-oxoazetidin-2-yl]phenyl}hex-5-enamide are dissolved in 6 ml of methanol. 0.1 N HCl(aq) is then added, and the mixture is stirred at room temperature overnight. The mixture is then neutralized with 1 N aqueous sodium hydroxide solution and concentrated using a rotary evaporator. The residue is stirred with dichloromethane and filtered and the mother liquor is concentrated using a rotary evaporator. The product is obtained following purification by preparative HPLC: C31H44F2N2O8 (682) MS (ESI): M+-18

後処理

  1. concentrationconcentrated
  2. customa rotary evaporator
  3. stirringThe residue is stirred with dichloromethane
  4. filtrationfiltered
  5. concentrationthe mother liquor is concentrated
  6. customa rotary evaporator
  7. customThe product is obtained
  8. custompurification by preparative HPLC

出典と根拠

ORDレコード
ord-d621314d504249e3b925ea9cb978f12d
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576200B2

反応ノート

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