Potassium bisulfate → tert-Butyl (4-oxopentyl)carbamate

HRID 1004257ノート

反応式

HRID 1004257 の反応式
[C:1]([O:5][C:6](=[O:17])[NH:7][CH2:8][CH2:9][CH2:10][C:11](=[O:16])N(OC)C)([CH3:4])([CH3:3])[CH3:2].[CH3:18][Mg]Br.OS([O-])(=O)=O.[K+]>C1COCC1>[C:1]([O:5][C:6](=[O:17])[NH:7][CH2:8][CH2:9][CH2:10][C:11](=[O:16])[CH3:18])([CH3:2])([CH3:3])[CH3:4]

参加物

5

反応物 3

HCID 516920Potassium bisulfateHCID 23112516tert-butyl N-(3-(methoxy(methyl)carbamoyl)propyl)carbamateHCID 178418573HCID 178418573、化合物

生成物 1

HCID 21478928tert-Butyl (4-oxopentyl)carbamate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 11-3 (10.0 g, 40.5 mmol) and THF (200 ml) at 0° C. was added methylmagnesium bromide (27.0 ml, 91.0 mmol; 3M in ether) dropwise over 20 minutes. After 2.0 hours, 10% KHSO4 was added slowly. The mixture was extracted with EtOAc. The organic portion was washed with sat. NaHCO3, brine, and dried over MgSO4. Evaporative removal of the solvent gave 11-4 as a colorless oil.

後処理

  1. extractionThe mixture was extracted with EtOAc
  2. washThe organic portion was washed with sat. NaHCO3, brine
  3. dry with materialdried over MgSO4
  4. customEvaporative removal of the solvent

出典と根拠

ORDレコード
ord-586ef15237fd46e596813bed9e2f94da
出典データセット
uspto-grants-2000_04
特許番号
US06048861

反応ノート

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