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Cyanuric chloride → HCID 23135159, 화합물

HRID 475517
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HRID 475517 반응식
[O:1]=[C:2]1[CH2:22][C:5]2[C:6]([C:19]([NH2:21])=O)=[N:7][N:8]([S:9]([C:12]3[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=3)(=[O:11])=[O:10])[C:4]=2[CH2:3]1.N1C(Cl)=NC(Cl)=NC=1Cl>CN(C=O)C>[O:1]=[C:2]1[CH2:22][C:5]2[C:6]([C:19]#[N:21])=[N:7][N:8]([S:9]([C:12]3[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=3)(=[O:11])=[O:10])[C:4]=2[CH2:3]1
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참가 물질

4

반응물 2

HCID 7954Cyanuric chlorideHCID 58713626HCID 58713626, 화합물

생성물 1

HCID 23135159HCID 23135159, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of the intermediate from step E above (0.91 mmol) in anhydrous DMF (5 mL) was added cyanuric chloride (334 mg, 2.0 mmol) in two portions. After stirring at room temperature for 15 minutes, the reaction was quenched by pouring into water (10 mL). The resulting mixture was extracted with ethyl acetate, washed with saturated NaHCO3, brine, dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO2) using 25% ethyl acetate-hexaries. A white solid was obtained.

후처리

  1. customthe reaction was quenched
  2. additionby pouring into water (10 mL)
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. washwashed with saturated NaHCO3, brine
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by flash chromatography (SiO2)
  9. customA white solid was obtained

출처 및 근거

ORD 기록
ord-f7d9d95a54484a388c76e41abb86cf62
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637555B2

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