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Iodoethane → HCID 9836705, 화합물

HRID 1057364
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HRID 1057364 반응식
[C:1]([O:5][C:6]([CH:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[CH:16][C:17]([O:19][CH3:20])=[CH:18][C:11]=2[NH:10][C:9]1=[O:21])=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:22](I)[CH3:23].C([O-])([O-])=O.[Cs+].[Cs+]>C(#N)C>[C:1]([O:5][C:6]([CH:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[CH:16][C:17]([O:19][CH3:20])=[CH:18][C:11]=2[N:10]([CH2:22][CH3:23])[C:9]1=[O:21])=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 10796Cesium carbonateHCID 9857210HCID 9857210, 화합물

생성물 1

HCID 9836705HCID 9836705, 화합물수율 88%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A suspension of 3(R,S)-tert-butoxycarbonyl-8-methoxy-2,3,4,5-tetrahydro-1H-1-benzazepine-2-one (3.645 g, 12.51 mmol), ethyl iodide (2.01 mL, 25.02 mmol) and Cs2CO3 (8.153 g, 25.02 mmol) in acetonitrile (35 mL) was stirred at room temperature for 6 hrs. The reaction mixture was evaporated to dryness, the residue dissolved in water and extracted with DCM. The organic layer was washed with water, dried over Na2SO4, filtered and evaporated to dryness. The solid residue was washed with n-hexane and dried in vacuum. The desired compound (3.50 g, 88%) was obtained as white crystalline powder.

후처리

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionthe residue dissolved in water
  3. extractionextracted with DCM
  4. washThe organic layer was washed with water
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness
  8. washThe solid residue was washed with n-hexane
  9. customdried in vacuum

출처 및 근거

ORD 기록
ord-156503904e64450f998d2edcc2d98a94
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06514965B1

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