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Pyridine → HCID 86665540, 화합물

HRID 1770749
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HRID 1770749 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH2:8][C:7]([CH3:10])([CH3:9])[NH:6][C:5]1=[O:11].N1C=CC=CC=1.[CH3:18][S:19](Cl)(=[O:21])=[O:20]>ClCCl>[CH3:18][S:19]([O:1][CH2:2][CH2:3][N:4]1[CH2:8][C:7]([CH3:9])([CH3:10])[NH:6][C:5]1=[O:11])(=[O:21])=[O:20]
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 67509984HCID 67509984, 화합물

생성물 1

HCID 86665540HCID 86665540, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 1-(2-hydroxyethyl)-4,4-dimethylimidazolidin-2-one (5.9 g, 37 mmol) and pyridine (3.6 mL, 44.4 mmol) in 150 mL of anhydrous dichloromethane was added methanesulfonyl chloride (3.3 mL, 43 mmol). The reaction was stirred at room temperature for 20 hours, then diluted with 100 mL of dichlormethane and washed twice with 40 mL of 1 N HCl and once with brine. The organic fraction was dried over sodium sulfate and concentrated in vacuo to 3.54 g of the desired product as white solid. 1H NMR (CDCl3, 400 MHz) δ 1.33 (s, 6H), 3.06 (s, 3H), 3.23 (s, 2H), 3.54-3.57 (t, J=5.2, 2H), 4.36-4.39 (t, J=5.2 Hz, 2H); LRMS (ESI/APCI) m/z 237 [M+H]+.

후처리

  1. washwashed twice with 40 mL of 1 N HCl and once with brine
  2. dry with materialThe organic fraction was dried over sodium sulfate
  3. concentrationconcentrated in vacuo to 3.54 g of the desired product as white solid

출처 및 근거

ORD 기록
ord-3a703f89dbc74e0db58f9c7a5f7eb60f
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09248117B2

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