Hydrochloric Acid → HCID 17976006、化合物

HRID 2264517ノート

反応式

HRID 2264517 の反応式
N[C:2]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:18]=[CH:17][C:13]3[O:14][CH2:15][O:16][C:12]=3[CH:11]=2)[C:5]([C:19]#[N:20])=[C:4]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:3]=1.N(OCCC(C)C)=O.[ClH:37]>C(#N)C.[Cu]Cl>[Cl:37][C:2]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:18]=[CH:17][C:13]3[O:14][CH2:15][O:16][C:12]=3[CH:11]=2)[C:5]([C:19]#[N:20])=[C:4]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:3]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 9799503HCID 9799503、化合物

生成物 1

HCID 17976006HCID 17976006、化合物

試薬・触媒・溶媒 2

HCID 62652Cuprous chloride触媒HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

400 mg (1.08 mmol) of 2-amino-4-(1,3-benzodioxol-5-yl)-6-benzyloxy-3,5-pyridinedicarbonitrile (example 1) are dissolved in 10 ml of acetonitrile. 759 mg (0.87 ml, 6.48 mmol) of isoamyl nitrite and 871 mg (6.48 mmol) of copper(I) chloride are then added, and the mixture is stirred at 40° C. for about 16 h. The reaction solution is then diluted with 1N hydrochloric acid and extracted three times with in each case 50 ml of dichloromethane. The combined organic phases are dried with sodium sulfate and concentrated under reduced pressure. The concentration residue is crystallized from dichloromethane/methanol.

後処理

  1. extractionextracted three times with in each case 50 ml of dichloromethane
  2. dry with materialThe combined organic phases are dried with sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe concentration residue is crystallized from dichloromethane/methanol

出典と根拠

ORDレコード
ord-6adaf7ac4ba840e48a1c445a12840026
出典データセット
uspto-grants-2010_12
特許番号
US07855219B2

反応ノート

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