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Hydrazine → HCID 21912822, 화합물

HRID 1245597
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HRID 1245597 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=O)[CH:15]([CH3:20])[C:16](=O)[O:17]C)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:22][NH2:23]>C1(C)C=CC=CC=1>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[NH:23][NH:22][C:16](=[O:17])[C:15]=2[CH3:20])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 21912726HCID 21912726, 화합물

생성물 1

HCID 21912822HCID 21912822, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 419 mg (1.4 mmol) of 1-(tert-butoxycarbonyl)-4-(1,3-dioxo-3-methoxy-2-methyl-prop-1-yl)piperidine (from Step B) and 0.26 mL (8.4 mmol) of hydrazine in 5 mL of toluene was refluxed for 50 minutes. The reaction was cooled to rt and placed in the freezer overnight. After decanting the solvent, the white solid was triturated with Et2O to provide the title compound, which was used without further purification. 1H-NMR (500 MHz) δ 1.49 (s, 9H), 1.55–1.63 (m, 2H), 1.77–1.79 (m, 2H), 1.90 (s, 3H), 2.69–2.77 (m, 3H), 4.22 (m, 2H), 5.15–5.79 (br m, 2H).

후처리

  1. customplaced in the freezer overnight
  2. customAfter decanting the solvent
  3. customthe white solid was triturated with Et2O

출처 및 근거

ORD 기록
ord-acca46599e064ab5b1b2484cec7067c1
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07125887B2

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