Dimethylformamide → 2-Phenyl-4-methyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile

HRID 68539노트

반응식

HRID 68539 반응식
[C:1]1([N:7]2[C:12](=[O:13])[NH:11][C:10](=[O:14])[C:9]([C:15]#[N:16])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:17]N(C=O)C.[H-].[Na+].CI>O>[C:1]1([N:7]2[C:12](=[O:13])[N:11]([CH3:17])[C:10](=[O:14])[C:9]([C:15]#[N:16])=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 563387HCID 563387, 화합물

생성물 1

HCID 47801582-Phenyl-4-methyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile수율 80%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Intermediate c (9 g, 0.042 mol) was added to DMF (100 mL). To the mixture was added NaH (1.3 g, 0.054 mol) in batch under an ice bath. After stirring for 30 min, methyl iodide (2.74 mL, 0.042 mol) was added dropwise. After the dropwise addition, the reaction was conducted for 2 h. After completion of the reaction, the reaction solution was poured into water (600 mL). A great deal of red solid separated out and was filtered by suction. The filtered cake was washed with water and dried to produce an orange red solid (7.6 g) in a yield of 80.0%.

후처리

  1. additionAfter the dropwise addition
  2. waitthe reaction was conducted for 2 h
  3. customAfter completion of the reaction
  4. customA great deal of red solid separated out
  5. filtrationwas filtered by suction
  6. washThe filtered cake was washed with water
  7. customdried

출처 및 근거

ORD 기록
ord-75a9f9c9efbb4141990b29869d1c0bb4
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822465B2

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