Triethylamine → tert-Butyl methylsulfonylcarbamate

HRID 711996노트

반응식

HRID 711996 반응식
C(N(CC)CC)C.[C:8]([O:12][C:13]([O:15]C(OC(C)(C)C)=O)=O)([CH3:11])([CH3:10])[CH3:9].[CH3:23][S:24]([NH2:27])(=[O:26])=[O:25]>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:23][S:24]([NH:27][C:13](=[O:15])[O:12][C:8]([CH3:11])([CH3:10])[CH3:9])(=[O:26])=[O:25]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 72879MethanesulfonamideHCID 90495Di-tert-butyl dicarbonate

생성물 1

HCID 10081367tert-Butyl methylsulfonylcarbamate수율 64.8%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

Triethylamine (2.2 mL, 16 mmol), di-tert-butyldicarbonate (2.65 g, 12.1 mmol) and 4-dimethylaminopyridine (0.096 g, 0.79 mmol) were added sequentially to a solution of methanesulfonamide (0.75 g, 7.9 mmol) in methylene chloride (20 mL) at room temperature. The reaction was stirred at room temperature for 2 h and then concentrated. EtOAc was added, and the resultant mixture was washed with 1N aq. HCl solution, dried over MgSO4 and concentrated to give the desired product (1 g) to be used in the next step directly.

후처리

  1. concentrationconcentrated
  2. additionEtOAc was added
  3. washthe resultant mixture was washed with 1N aq. HCl solution
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-836d82747f414104877ffad99140d64a
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181271B2

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