Water → HCID 22246914, 화합물

HRID 1595834노트

반응식

HRID 1595834 반응식
[CH2:1]([C:5]1[CH:12]=[CH:11][C:8]([CH2:9][NH2:10])=[CH:7][CH:6]=1)[CH2:2][CH2:3][CH3:4].N1C=CC=CC=1.[CH3:19][S:20](Cl)(=[O:22])=[O:21].O>C(Cl)Cl>[CH2:1]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][NH:10][S:20]([CH3:19])(=[O:22])=[O:21])=[CH:11][CH:12]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 40298714-Butylbenzylamine

생성물 1

HCID 22246914HCID 22246914, 화합물수율 57.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-butylbenzylamine (4.01 g, 24.6 mmol) in CH2Cl2 (75 mL) was added pyridine (4.0 mL, 49 mmol) followed by dropwise addition of methanesulfonyl chloride (2.5 mL, 32.3 mmol). The reaction was stirred at room temperature for 24 h and water was added. The product was extracted into CH2Cl2 (2×) and the organic solution was dried (MgSO4), filtered, and concentrated. Flash chromatography (2:1 to 1:1 hexanes:EtOAc) provided the title compound as a white solid (3.4114 g). 1H NMR (400 MHz, CDCl3) δ 7.23 (d, 2H), 7.15 (d, 2H), 4.84 (m, 1H), 4.25 (d, 2H), 2.82 (s, 3H), 2.58 (t, 2H), 1.56 (m, 2H), 1.33 (m, 2H), 0.91 (t, 3H).

후처리

  1. extractionThe product was extracted into CH2Cl2 (2×)
  2. dry with materialthe organic solution was dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a304cf5ed65c485381636817aeabc0dd
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06288120B1

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