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2,6-Lutidine → 1-(2-(Trimethylsilyl)ethyl) 1'-tert-butyl 5-formylspiro[indoline-3,3'-pyrrolidine]-1,1'-dicarboxylate

HRID 1411308
ノート
印刷プレビュー

反応式

HRID 1411308 の反応式
[CH:1]([C:3]1[CH:4]=[C:5]2[C:11]3([CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12]3)[CH2:10][N:9]([C:23]([O:25][CH2:26][CH2:27][Si:28]([CH3:31])([CH3:30])[CH3:29])=[O:24])[C:6]2=[CH:7][CH:8]=1)=C.I([O-])(=O)(=O)=[O:33].[Na+].N1C(C)=CC=CC=1C.S([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.[Os](=O)(=O)(=O)=O.O>[CH:1]([C:3]1[CH:4]=[C:5]2[C:11]3([CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:21])([CH3:22])[CH3:20])=[O:17])[CH2:12]3)[CH2:10][N:9]([C:23]([O:25][CH2:26][CH2:27][Si:28]([CH3:31])([CH3:30])[CH3:29])=[O:24])[C:6]2=[CH:7][CH:8]=1)=[O:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 79372,6-LutidineHCID 24437Sodium SulfiteHCID 23667635Sodium periodateHCID 90449481HCID 90449481、化合物

生成物 1

HCID 904497561-(2-(Trimethylsilyl)ethyl) 1'-tert-butyl 5-formylspiro[indoline-3,3'-pyrrolidine]-1,1'-dicarboxylate収率 82%

試薬・触媒・溶媒 3

HCID 30318
Osmium Tetroxide
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

実験手順

1-(2-(Trimethylsilyl)ethyl) 1′-tert-butyl 5-vinylspiro[indoline-3,3′-pyrrolidine]-1,1′-dicarboxylate (674 mg, 1.52 mmol) was dissolved in dioxane (15 mL). Thereafter, sodium periodate (1.30 g, 6.08 mmol), water (5 mL), 2,6-lutidine (0.35 mL, 3.01 mmol), and osmium tetroxide (1% t-butanol aqueous solution, 1 mL) were added to the above obtained solution under cooling on ice, and the thus obtained mixture was then stirred at the same temperature as above for 3 hours. Thereafter, an aqueous solution of sodium sulfite was added to the reaction solution, and the mixture was then extracted with chloroform. The organic layer was washed with brine, and was then dried over anhydrous sodium sulfate, followed by concentration in vacuo. The obtained residue was purified by silica gel column chromatography (hexane ethyl acetate=5:1) to obtain 1-(2-(trimethylsilyl)ethyl) 1′-tert-butyl 5-formylspiro[indoline-3,3′-pyrrolidine]-1,1′-dicarboxylate (553 mg, 82%) in the form of a light yellow solid.

後処理

  1. temperatureunder cooling on ice
  2. extractionthe mixture was then extracted with chloroform
  3. washThe organic layer was washed with brine
  4. dry with materialwas then dried over anhydrous sodium sulfate
  5. concentrationfollowed by concentration in vacuo
  6. customThe obtained residue was purified by silica gel column chromatography (hexane ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-424e45b2085e450fb6fd2c1dc148be2a
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921576B2

反応ノート

読み込み中…

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