Triethylamine → tert-butyl {[((2R)-1,4-dioxan-2-ylmethyl)(methyl)amino]sulfonyl}carbamate

HRID 1987100노트

반응식

HRID 1987100 반응식
Cl.[O:2]1[CH2:7][CH2:6][O:5][CH2:4][CH:3]1[CH2:8][NH:9][CH3:10].[C:11]([O:15][C:16]([NH:18][S:19](N1C=CC(=[N+](C)C)C=C1)(=[O:21])=[O:20])=[O:17])([CH3:14])([CH3:13])[CH3:12].C(N(CC)CC)C>ClCCl>[O:2]1[CH2:7][CH2:6][O:5][CH2:4][C@H:3]1[CH2:8][N:9]([CH3:10])[S:19]([NH:18][C:16](=[O:17])[O:15][C:11]([CH3:13])([CH3:12])[CH3:14])(=[O:20])=[O:21]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 66972118(1,4-Dioxan-2-ylmethyl)methylamine hydrochlorideHCID 178482963HCID 178482963, 화합물

생성물 1

HCID 53309829tert-butyl {[((2R)-1,4-dioxan-2-ylmethyl)(methyl)amino]sulfonyl}carbamate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-(1,4-dioxan-2-yl)-N-methylmethanamine hydrochloride (0.760 g, 4.55 mmol), N-[1-{[(tert-butoxycarbonyl)amino]sulfonyl}pyridin-4(1H)-ylidene]-N-methylmethanaminium (1.51 g, 5.00 mmol), and triethylamine (1.55 mL, 11.4 mmol) were slurried in 50 mL dichloromethane and stirred at ambient temperature. After 12 hours, the solution was concentrated in vacuo and purified by silica chromatography (50-100% ethyl acetate/hexanes gradient) to afford the title compound. LRMS (APCI) calc'd for (C11H22N2O6SNa) [M+Na]+, 333.1; found, 333.1.

후처리

  1. concentrationthe solution was concentrated in vacuo
  2. custompurified by silica chromatography (50-100% ethyl acetate/hexanes gradient)

출처 및 근거

ORD 기록
ord-2672778e0eee457c9cc1f36f41bb9933
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07550478B2

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