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Cyanuric chloride → HCID 57916539, 화합물

HRID 1040496
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HRID 1040496 반응식
[CH2:1]([O:8][C:9](=[O:17])[NH:10][C:11]1([C:14](=O)[NH2:15])[CH2:13][CH2:12]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]([O:8][C:9](=[O:17])[NH:10][C:11]1([C:14]#[N:15])[CH2:13][CH2:12]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7954Cyanuric chlorideHCID 13676801(1-Carbamoyl-cyclopropyl)-carbamic acid benzyl ester

생성물 1

HCID 57916539HCID 57916539, 화합물수율 84.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a 0° C. solution of (1-carbamoyl-cyclopropyl)-carbamic acid benzyl ester (1.8 g, 7.7 mmol) in DMF (20 mL) was added cyanuric chloride in one portion. The reaction was allowed to warm to room temperature overnight. The reaction was quenched with water and extracted with EtOAc (3×100 mL). The combined extracts were washed with water (3×50 mL), brine and dried with MgSO4. The mixture was filtered and concentrated. The resulting crude residue was dissolved in 30% EtOAc in hexanes (90 mL) and filtered through a plug of silica gel. The filtrate was concentrated to give (1-cyano-cyclopropyl)-carbamic acid benzyl ester (1.4 g, 6.5 mmol) as a white foam.

후처리

  1. customThe reaction was quenched with water
  2. extractionextracted with EtOAc (3×100 mL)
  3. washThe combined extracts were washed with water (3×50 mL), brine
  4. dry with materialdried with MgSO4
  5. filtrationThe mixture was filtered
  6. concentrationconcentrated
  7. dissolutionThe resulting crude residue was dissolved in 30% EtOAc in hexanes (90 mL)
  8. filtrationfiltered through a plug of silica gel
  9. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-8dd9570f492d4028a1bf4af76aa5410e
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08552205B2

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