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

HRID 1004257노트

반응식

HRID 1004257 반응식
[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]

참가 물질

5

반응물 3

HCID 516920Potassium bisulfateHCID 23112516tert-butyl N-(3-(methoxy(methyl)carbamoyl)propyl)carbamateHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 21478928tert-Butyl (4-oxopentyl)carbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-586ef15237fd46e596813bed9e2f94da
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06048861

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