tert-Butanol → 1-cyclopropyl-8-(1-Bocamino-1-cyclopropyl)-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid ethyl ester

HRID 1900

反応式

HRID 1900 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[N:14]2[C:9]([C:10]([CH3:24])=[C:11]([C:18]3(C(O)=O)[CH2:20][CH2:19]3)[C:12]([F:17])=[CH:13]2)=[C:8]([CH:25]2[CH2:27][CH2:26]2)[CH:7]=1)=[O:5])[CH3:2].C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:35])C=CC=CC=1.[C:45]([OH:49])([CH3:48])([CH3:47])[CH3:46].C([N:52]([CH2:55]C)CC)C>O1CCOCC1>[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[N:14]2[C:9]([C:10]([CH3:24])=[C:11]([C:18]3([NH:52][C:55]([O:49][C:45]([CH3:48])([CH3:47])[CH3:46])=[O:35])[CH2:19][CH2:20]3)[C:12]([F:17])=[CH:13]2)=[C:8]([CH:25]2[CH2:26][CH2:27]2)[CH:7]=1)=[O:5])[CH3:2]

参加物

6

反応物 4

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 571289751-cyclopropyl-8-(1-hydroxycarbonyl-1-cyclopropyl)-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid ethyl ester

生成物 1

HCID 571023201-cyclopropyl-8-(1-Bocamino-1-cyclopropyl)-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A sample of the product from Step 477d is heated with diphenylphosphoryl azide, t-butanol, triethylamine and dioxane. The solvents is removed under vacuum. The residue is dissolved in methylene chloride, washed with water and dried over MgSO4 and concentrated under vacuum. The title compound is purified by chromatography on silica gel.

後処理

  1. customThe solvents is removed under vacuum
  2. dissolutionThe residue is dissolved in methylene chloride
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under vacuum
  6. customThe title compound is purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-e9a35b5778f84e018ef46a7daf51dbfd
出典データセット
uspto-grants-1998_03
特許番号
US05726182

関連ノート

読み込み中…