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Water → tert-butyl N-(4-methyl-1-oxopentan-2-yl)carbamate

HRID 2401256
ノート
印刷プレビュー

反応式

HRID 2401256 の反応式
[OH:1][CH2:2][CH:3]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:4][CH:5]([CH3:7])[CH3:6].I(C1C=CC=CC=1C(O)=O)(=O)=O.O>CS(C)=O>[CH3:6][CH:5]([CH3:7])[CH2:4][CH:3]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:2]=[O: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 962WaterHCID 1087942-Iodoxybenzoic acidHCID 546110tert-butyl N-(1-hydroxy-4-methylpentan-2-yl)carbamate

生成物 1

HCID 546109tert-butyl N-(4-methyl-1-oxopentan-2-yl)carbamate

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a solution of tert-butyl (1-hydroxy-4-methylpentan-2-yl)carbamate (2.7 g) in DMSO (60 mL) was added 2-iodoxybenzoic acid (3.5 g), and the mixture was stirred at room temperature for 3 hr. Water was added thereto, the resulting insoluble matter was filtered off, and the filtrate was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. After the dessicant was filtered off, the filtrate was concentrated under reduced pressure to afford a crude product of tert-butyl (4-methyl-1-oxopentan-2-yl)carbamate.

後処理

  1. filtrationthe resulting insoluble matter was filtered off
  2. extractionthe filtrate was extracted with ethyl acetate
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationAfter the dessicant was filtered off
  6. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-1068b36a8d4649d2b34630d4b93a9902
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08796272B2

反応ノート

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