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

HRID 2289158ノート

反応式

HRID 2289158 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 1-3 (10.0 g, 40.5 mmol) and THF (200 ml) at 0° C. was added methyl magnesium bromide (27.0 ml, 91.0 mmol; 3M in ether) dropwise over 20 minutes. Mter 2.0 hours, 10% KHSO4 was added slowly. The mixture was extracted with EtOAc. The organic portion was washed with saturated NaHCO3, brine, and dried over MgSO4. Evaporative removal of the solvent gave 1-4 as a colorless oil.

後処理

  1. extractionThe mixture was extracted with EtOAc
  2. washThe organic portion was washed with saturated 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-696f3cf5a37a4ce09e24f18fba1559ba
出典データセット
uspto-grants-2000_07
特許番号
US06090944

反応ノート

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