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Triethylamine → 1-Oxa-3-azaspiro(4.5)decan-2-one

HRID 1710398
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HRID 1710398 반응식
Cl.[NH2:2][CH2:3][C:4]1([OH:10])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.C(N(CC)CC)C.N1C=CC=C[C:19]=1[O:24]C(=O)OC1C=CC=CN=1>ClCCl.C(OCC)(=O)C>[O:10]1[C:4]2([CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]2)[CH2:3][NH:2][C:19]1=[O:24]
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 2757370Carbonic acid di-2-pyridyl esterHCID 3084332Cyclohexanol, 1-(aminomethyl)-, hydrochloride (1:1)

생성물 1

HCID 3490431-Oxa-3-azaspiro(4.5)decan-2-one수율 74.7%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857
Ethyl Acetate
용매

실험 절차

1-Aminomethyl-cyclohexanol hydrogen chloride (250 mg, 1.5 mmol) and triethylamine (0.21 mL, 1.5 mmol) were mixed in dichloromethane (5 mL), and the mixture was stirred for 15 min. Carbonic acid dipyridin-2-yl ester (326 mg, 1.5 mmol) was then added, and the reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate (10 mL), washed with water (2×4 mL), brine (2×4 mL); dried over anhydrous sodium sulfate and concentrated to give the title compound as a white powder (174 mg, 74%). 1H NMR (300 MHz, CDCl3): δ 6.42 (br, 1H), 3.31 (s, 2H), 1.86 (m, 2H), 1.76 (m, 2H), 1.65 (m, 2H), 1.47 (m, 4H).

후처리

  1. stirringthe reaction mixture was stirred at room temperature overnight
  2. washwashed with water (2×4 mL), brine (2×4 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ec4b05dd8e134ff9bc76840b8f706163
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790717B2

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