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Tert-Butyl hypochlorite → HCID 54582542, 화합물

HRID 1770746
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HRID 1770746 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][C:8]([CH3:11])([CH3:10])[NH:7][C:6]([CH3:13])([CH3:12])[C:5]1=[O:14].C(O[Cl:20])(C)(C)C>CO>[Cl:20][N:7]1[C:8]([CH3:10])([CH3:11])[CH2:9][N:4]([CH2:3][CH2:2][OH:1])[C:5](=[O:14])[C:6]1([CH3:13])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 521297Tert-Butyl hypochloriteHCID 21951121HCID 21951121, 화합물

생성물 1

HCID 54582542HCID 54582542, 화합물수율 75.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1-(2-hydroxyethyl)-3,3,5,5-tetramethylpiperazin-2-one (125 mg, 0.63 mmol) in methanol (1 ml) was cooled to 0° C. tert-Butylhypochlorite (106 ul, 0.94 mmol) was added. The resulting solution was stirred for 60 minutes, and then concentrated under reduced pressure. The crude material was purified by column chromatography eluting from silica gel with a gradient of 0-8% methanol in dichloromethane to give 111 mg of a white solid. 1H NMR (D2O, 400 MHz) δ 1.21 (s, 3H), 1.43 (s, 3H), 3.36 (s, 2H), 3.43-3.345 (t, J=5.6 Hz, 2H), 3.64-3.66 (t, J=5.6 Hz, 2H). 13C NMR (D2O, 100 MHz) δ 172.9, 68.1, 60.0, 58.4, 57.4, 49.6, 25.5, 22.7. LRMS (ESI/APCI) m/z 235 [M+H]+.

후처리

  1. additionwas added
  2. concentrationconcentrated under reduced pressure
  3. customThe crude material was purified by column chromatography
  4. washeluting from silica gel with a gradient of 0-8% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-ac061659e0a7400893080feea8439cac
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09248117B2

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