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1,1'-Carbonyldiimidazole → HCID 118308695、化合物

HRID 923492
ノート
印刷プレビュー

反応式

HRID 923492 の反応式
[C:1]([O:5][C:6]([N:8]1[C:12]([CH3:16])([C:13]([OH:15])=O)[CH2:11][O:10][C:9]1([CH3:18])[CH3:17])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(N1C=CN=C1)(N1C=CN=C1)=O.O[NH:32][C:33](=[NH:35])[CH3:34]>CN(C=O)C>[CH3:17][C:9]1([CH3:18])[N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[C:12]([CH3:16])([C:13]2[O:15][N:35]=[C:33]([CH3:34])[N:32]=2)[CH2:11][O:10]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 682631,1'-CarbonyldiimidazoleHCID 230022953-(tert-Butoxycarbonyl)-2,2,4-trimethyloxazolidine-4-carboxylic acidHCID 178465666HCID 178465666、化合物

生成物 1

HCID 118308695HCID 118308695、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 430 mg of 3-(tert-butoxycarbonyl)-2,2,4-trimethyl-1,3-oxazolidine-4-carboxylic acid in 4 ml of DMF was added 296 mg of 1,1′-carbonyldiimidazole, followed by stirring at room temperature for 2 hours. To the reaction mixture was added 146 mg of N-hydroxyacetamidine, followed by stirring at room temperature for 1 hour, at 110° C. for 2 hours, and then at 130° C. overnight. The reaction mixture was left to be cooled to room temperature and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 390 mg of tert-butyl 2,2,4-trimethyl-4-(3-methyl-1,2,4-oxadiazol-5-yl)-1,3-oxazolidine-3-carboxylate.

後処理

  1. stirringby stirring at room temperature for 1 hour, at 110° C. for 2 hours
  2. customat 130° C.
  3. customovernight
  4. waitThe reaction mixture was left
  5. temperatureto be cooled to room temperature
  6. customthe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-4203084bff3e43d0a95a245939dd47d5
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278968B2

反応ノート

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