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

HRID 1061718
ノート
印刷プレビュー

反応式

HRID 1061718 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d313c438859e41a984e2dbc8b1c7a778
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06960594B2

反応ノート

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