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Ethylenediamine → 2-(2-Aminoethyl)-1,3-di-Boc-guanidine

HRID 1061718
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HRID 1061718 반응식
[C:1]([NH:8][C:9]([N:18]1[CH:22]=[CH:21]C=N1)=[N:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N)C[NH2:25]>C1COCC1>[C:11]([NH:10][C:9]([NH:8][C:1]([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2])=[N:18][CH2:22][CH2:21][NH2:25])([O:13][C:14]([CH3:15])([CH3:16])[CH3:17])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 4428040N,N'-Bis(tert-butoxycarbonyl)-1H-pyrazole-1-carboxamidine

생성물 1

HCID 109903042-(2-Aminoethyl)-1,3-di-Boc-guanidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

With continued reference to Scheme J, a solution of the N,N′-bis-(Boc)-1H-Pyrazole-1-carboxamidine (2 g, 6.45 mmol) in THF (50 ml) was added dropwise to ethylene diamine (4 ml, 59.6 mmol) in THF (100 ml). After 30 min of mixing at room temperature solvent was evaporated then toluene (100 ml) was added and evaporated in order to remove remaining traces of the ethylene diamine. The resulting product (Compound XXIV) was treated immediately according to scheme K since it decomposes at room temperature. 1H NMR (CDCl3, 400 MHz) δ 1.40-1.61 (m, 18H), 2.87-2.90 (t, 2H,), 3.47-3.50 (m, 2H), 6.31-6.34 (t, 0.61H), 7.61-7.62 (d, 1H), 8.45-8.66 (broad s).

후처리

  1. additionAfter 30 min of mixing at room temperature solvent
  2. customwas evaporated
  3. additiontoluene (100 ml) was added
  4. customevaporated in order
  5. customto remove
  6. additionThe resulting product (Compound XXIV) was treated immediately
  7. customdecomposes at room temperature

출처 및 근거

ORD 기록
ord-d313c438859e41a984e2dbc8b1c7a778
출처 데이터셋
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06960594B2

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