Diisopropylethylamine → 1,1-Dimethylethyl 2-[[(methylsulfonyl)oxy]methyl]-2-(hydroxymethyl)-4-morpholinecarboxylate

HRID 2110803노트

반응식

HRID 2110803 반응식
[OH:1][CH2:2][CH:3]1[O:8][CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1.C(N(C(C)C)C(C)C)C.[CH3:25][S:26]([O:29]S(C)(=O)=O)(=O)=[O:27].[C:34]([O-])(O)=[O:35].[Na+]>ClCCl>[CH3:25][S:26]([O:1][CH2:2][C:3]1([CH2:34][OH:35])[O:8][CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1)(=[O:29])=[O:27]

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 81560Methanesulfonic anhydrideHCID 516892Sodium BicarbonateHCID 5201202tert-Butyl 2-(hydroxymethyl)morpholine-4-carboxylate

생성물 1

HCID 866286481,1-Dimethylethyl 2-[[(methylsulfonyl)oxy]methyl]-2-(hydroxymethyl)-4-morpholinecarboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of (2S) 1,1-dimethylethyl 2-(hydroxymethyl)-4-morpholinecarboxylate (5.63 g) (Heterocycles, 1993, 35, 105) and N-ethyl-N,N-diisopropylamine (9 ml) in dichloromethane (200 ml) at room temperature was added methanesulfonic anhydride (5.42 g). The reaction was stirred for 16 hours. The reaction mixture was poured onto saturated aqueous NaHCO3 solution and the organics were extracted with dichloromethane. The combined organic extracts were dried with MgSO4 and concentrated to give an oil (8.33 g). This was used without further purification.

후처리

  1. extractionthe organics were extracted with dichloromethane
  2. dry with materialThe combined organic extracts were dried with MgSO4
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-832497995f604c21b3b3cc20dc7cf4d4
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517989B2

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