Hydrochloric Acid → HCID 17976006, 화합물

HRID 2264517노트

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HRID 2264517 반응식
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

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 9799503HCID 9799503, 화합물

생성물 1

HCID 17976006HCID 17976006, 화합물

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매HCID 6342Acetonitrile용매

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온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6adaf7ac4ba840e48a1c445a12840026
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07855219B2

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