Methanol → HCID 178471968, 화합물

HRID 240312

반응식

HRID 240312 반응식
[CH2:1]([O:3][C:4](=[O:8])[CH2:5][C:6]#[N:7])[CH3:2].[H-].[Na+].[O:11]=[C:12]1[C:24]2[C:19](=[N:20][C:21](C#N)=[C:22]([C:25]#[N:26])[N:23]=2)[C:18]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]1=2.CO>CN(C=O)C>[C:6]([C:5]([C:21]1[N:20]=[C:19]2[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[C:12](=[O:11])[C:24]2=[N:23][C:22]=1[C:25]#[N:26])=[C:4]([O:3][CH2:1][CH3:2])[OH:8])#[N:7]

참가 물질

6

반응물 4

HCID 887MethanolHCID 7764Ethyl cyanoacetateHCID 24758Sodium hydrideHCID 2929299-oxo-9H-indeno(1,2-b)pyrazine-2,3-dicarbonitrile

생성물 1

HCID 178471968HCID 178471968, 화합물수율 97.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

Ethylcyanoacetate (110 mg, 0.970 mmol) was dissolved, under inert atmosphere, in dry DMF (1 ml) and NaH (39 mg, 0.970 mmol) was added in one portion. After 30 min, a solution of 1 (150 mg, 0.646 mmol) in dry DMF (2 ml) was added dropwise. After 15 min MeOH was added and the solution stirred for 10 min. The solvents were evaporated and the crude purified by flash chromatography (EtOAc:MeOH 9:1) affording 22 as a dark red solid (200 mg, 97%).

후처리

  1. customThe solvents were evaporated
  2. customthe crude purified by flash chromatography (EtOAc:MeOH 9:1)

출처 및 근거

ORD 기록
ord-acdda630ff26422c8d67586bdcbc4117
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648076B2

연결된 노트

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