Cyanuric chloride → HCID 23135168, 화합물

HRID 475507노트

반응식

HRID 475507 반응식
[CH2:1]([N:8]1[C:12]2[CH2:13][C:14](=[O:16])[CH2:15][C:11]=2[C:10]([C:17]([NH2:19])=O)=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N1C(Cl)=NC(Cl)=NC=1Cl>CN(C=O)C>[CH2:1]([N:8]1[C:12]2[CH2:13][C:14](=[O:16])[CH2:15][C:11]=2[C:10]([C:17]#[N:19])=[N:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 7954Cyanuric chlorideHCID 58713637HCID 58713637, 화합물

생성물 1

HCID 23135168HCID 23135168, 화합물수율 76.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of the intermediate from step E (5.25 mmol) in DMF (60 mL) was added cyanuric chloride (3.12 g, 17 mmol) in three portions. After 30 minutes at room temperature, the reaction was quenched with water and extracted with ethyl acetate (2×). The organic layer was washed with water, brine and dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The residue was purified by flash chromatography (SiO2) using 30% ethyl acetate-hexanes to give the desired product (0.95 g) as a yellow solid.

후처리

  1. customthe reaction was quenched with water
  2. extractionextracted with ethyl acetate (2×)
  3. washThe organic layer was washed with water, brine
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash chromatography (SiO2)

출처 및 근거

ORD 기록
ord-8aeaa62b7ed34ef3a4ea97143e4939f0
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637555B2

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