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HRID237416

反应详情

EQUATION

反应方程式

HRID 237416 的结构方程式

REACTANTS

反应物

2
结构：C1CCC2=NCCCN2CC1
HCID81184

1,8-Diazabicyclo[5.4.0]undec-7-ene

C9H16N2

结构：CC(=O)O[C@H]1C(=O)[C@@]2(C)[C@H]([C@H](OC(=O)c3ccccc3)[C@]3(O)C[C@H](OC(=O)[C@H](O)[C@@H](NC(=O)c4ccccc4)c4ccccc4)C(C)=C1C3(C)C)[C@]1(OC(C)=O)CO[C@@H]1C[C@@H]2O.CC(C)(NCC(O)COc1cccc2[nH]c3ccccc3c12)c1ccc(N=[N+]=[N-])cc1.CC(C)C[C@H](NC(=O)OCC1c2ccccc2-c2ccccc21)C(=O)O
HCID131731173

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)O[C@H]1C(=O)[C@@]2(C)[C@H]([C@H](OC(=O)c3ccccc3)[C@]3(O)C[C@H](OC(=O)[C@H](O)[C@@H](NC(=O)c4ccccc4)c4ccccc4)C(C)=C1C3(C)C)[C@]1(OC(C)=O)CO[C@@H]1C[C@@H]2O.CC(C)(NCC(O)COc1cccc2[nH]c3ccccc3c12)c1ccc(N=[N+]=[N-])cc1.CC(C)C[C@H](N)C(=O)O
HCID131731175

未命名化合物

收率 84%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

8 (0.50 g, 0.37 mmol) was treated with 1% of 1,8-Diazabicyclo[5.4.0]undec-7-en (DBU) in Tetrahydrofuran (THF) (10 mL) for 45 seconds at room temperature and the product was precipitated by 1 M HCl in diethyl ether (500 mL). Then it was purified on a silica gel column using chloroform/methanol (7:1) to afford 9 (350 mg, 84%) as a white powder. ESI-MS (5 kV, MeOH): m/z (%)=1116.1 (100) [M+H]+; HPLC (230 nm): >95%.

WORKUP

后处理

  1. customthe product was precipitated by 1 M HCl in diethyl ether (500 mL)
  2. customThen it was purified on a silica gel column