Triethylamine → HCID 86657585、化合物
反応式
[C:1](NC1(C(O)=O)CC1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCN(CC)CC.CN(C(ON1[N:39]=[N:38][C:33]2[CH:34]=C[CH:36]=[N:37][C:32]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[C:47]([O:51][C:52](NN)=[O:53])([CH3:50])([CH3:49])[CH3:48].CC1C([O:63]C(C)=O)=CC(C(C)C)=C(OCC[NH+](C)C)C=1.[Cl-]>CN(C=O)C.O>[C:47]([O:51][C:52]([NH:39][NH:38][C:33]1([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:34][CH:32]1[N:37]=[C:36]=[O:63])=[O:53])([CH3:50])([CH3:49])[CH3:48]参加物
反応物 5
生成物 1
試薬・触媒・溶媒 2
実験手順
To a solution of 1-benzoylamino-cyclopropanecarboxylic acid (5.0 g, 21.3 mmol) in DMF (5 mL) was added Et3N (2.94 mL, 21.3 mmol) and HATU (8.08 g, 21.3 mmol). The reaction mixture was allowed to stir for 10 min then hydrazinecarboxylic acid tert-butyl ester (2.81 g, 21.3 mmol) was added. The reaction was allowed to stir at room temperature overnight. The mixture was diluted with water and extracted with EtOAc (3×50 mL). The combined extracts were washed with saturated NaHCO3, 2N HCl, brine and dried with MgSO4. The mixture was filtered, concentrated in vacuo, and purified by silica gel chromatography (25-100% EtOAc in hexanes) to give the N′-(1-benzyloxy-carbonylamino-cyclopropyl)-hydrazinecarboxylic acid tert-butyl ester (6.2 g, 17.7 mmol) as a white solid, m/z 250.6 [M−101]+.
後処理
- stirringto stir at room temperature overnight
- extractionextracted with EtOAc (3×50 mL)
- washThe combined extracts were washed with saturated NaHCO3, 2N HCl, brine
- dry with materialdried with MgSO4
- filtrationThe mixture was filtered
- concentrationconcentrated in vacuo
- custompurified by silica gel chromatography (25-100% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-586980b88d01402ea2efb0e4950b4ec7
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08552205B2
反応ノート
読み込み中…