N,N'-羰基二咪唑 → Ngb-2849

HRID 1941455

反应方程式

HRID 1941455 反应方程式
[CH:1]1[C:14]2[C:5](=[CH:6][C:7]3[C:12]([CH:13]=2)=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:4]=[CH:3][C:2]=1[C:15](O)=[O:16].C(N1C=CN=C1)(N1C=CN=C1)=O.[Cl:30][C:31]1[C:36]([Cl:37])=[CH:35][CH:34]=[CH:33][C:32]=1[N:38]1[CH2:43][CH2:42][N:41]([CH2:44][CH2:45][CH2:46][CH2:47][NH2:48])[CH2:40][CH2:39]1>O1CCCC1>[Cl:30][C:31]1[C:36]([Cl:37])=[CH:35][CH:34]=[CH:33][C:32]=1[N:38]1[CH2:39][CH2:40][N:41]([CH2:44][CH2:45][CH2:46][CH2:47][NH:48][C:15]([C:2]2[CH:3]=[CH:4][C:5]3[C:14](=[CH:13][C:12]4[C:7]([CH:6]=3)=[CH:8][CH:9]=[CH:10][CH:11]=4)[CH:1]=2)=[O:16])[CH2:42][CH2:43]1

参与物

5

反应物 3

HCID 68263N,N'-羰基二咪唑HCID 1013252-蒽甲酸HCID 11098669阿立哌唑杂质1751

产物 1

HCID 15411150Ngb-2849收率 80.3%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂2 次

实验过程

A mixture of 2-anthracenecarboxylic acid (100 mg, 0.45 mmol) and 1,1'-carbonyldiimidazole (82 mg, 0.5 mmol) in 10 mL of anhydrous tetrahydrofuran is stirred for 8 hours. A solution of 4-[4-(2,3-dichlorophenyl)-1-piperazinyl]-1-aminobutane (150 mg, 0.5 mmol) in 1 mL of tetrahydrofuran is added and the resulting mixture is stirred for 30 minutes. The reaction mixture is partitioned between ethyl acetate and water. The organic layer is washed with aqueous Na2CO3, dried (Na2SO4) and concentrated in vacuo to give the title compound (183 mg, 80%). The hydrochloride salt is prepared by treating the free base with ethyl acetate-HCl. The hydrochloride salt of the title compound has a melting point of 245°-247° C.

后处理

  1. stirringthe resulting mixture is stirred for 30 minutes
  2. customThe reaction mixture is partitioned between ethyl acetate and water
  3. washThe organic layer is washed with aqueous Na2CO3
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo

来源与证据

ORD记录
ord-c3cc45258c624e9ea9407c2a0419ea4e
来源数据集
uspto-grants-1997_12
专利号
US05703235

关联笔记

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