二氯甲烷 → 7-Bromo-4-(4-chloro-2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinoline

HRID 8262

反应方程式

HRID 8262 反应方程式
S(Cl)(Cl)(=O)=O.Cl[CH2:7][Cl:8].[Br:9][C:10]1[CH:19]=[C:18]2[C:13]([C:14]([C:20]3[C:24]([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=4)=[N:23][N:22]4[CH2:31][CH2:32]C[C:21]=34)=[CH:15][CH:16]=[N:17]2)=[CH:12][CH:11]=1>N1C=CC=CC=1>[Br:9][C:10]1[CH:19]=[C:18]2[C:13]([C:14]([C:20]3[C:24]([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=4)=[N:23][N:22]4[CH2:31][CH2:32][CH:7]([Cl:8])[C:21]=34)=[CH:15][CH:16]=[N:17]2)=[CH:12][CH:11]=1

参与物

5

反应物 3

HCID 6344二氯甲烷HCID 24648磺酰氯HCID 219925197-bromo-4-(2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinoline

产物 1

HCID 101132117-Bromo-4-(4-chloro-2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinoline

试剂、催化剂与溶剂 1

HCID 1049吡啶溶剂

实验过程

A solution of 1 M sulfuryl chloride in dichloromethane (20 mL, 20 mmol) is added to a solution of 7-bromo-4-(2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinoline (2.2 g, 5.62 mmol) in dry pyridine (50 mL). The mixture is stirred for 18 h and concentrated in vacuo. The residue is partitioned between chloroform and saturated sodium chloride. The organic layer is dried (sodium sulfate), filtered, concentrated in vacuo, and the residue chromatographed on SiO2 (dichloromethane to 20% methanol in dichloromethane) to yield the title compound as a red solid, 1.8 g (75%).

后处理

  1. concentrationconcentrated in vacuo
  2. customThe residue is partitioned between chloroform and saturated sodium chloride
  3. dry with materialThe organic layer is dried (sodium sulfate)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customthe residue chromatographed on SiO2 (dichloromethane to 20% methanol in dichloromethane)

来源与证据

ORD记录
ord-5117de9338de4a369384dbd7fc1bb107
来源数据集
uspto-grants-2006_08
专利号
US07087626B2

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