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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dichloromethane → HCID 19936399, 화합물

HRID 36870
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HRID 36870 반응식
C(Cl)Cl.C[O:5][C:6]1[CH:21]=[CH:20][C:9]([CH2:10][N:11]2[NH:17][C:16](=[O:18])[CH:15]3[CH:13]([CH2:14]3)[C:12]2=[O:19])=[CH:8][CH:7]=1.B(Br)(Br)Br>O>[OH:5][C:6]1[CH:7]=[CH:8][C:9]([CH2:10][N:11]2[NH:17][C:16](=[O:18])[CH:15]3[CH:13]([CH2:14]3)[C:12]2=[O:19])=[CH:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 25134Boron tribromideHCID 107768063-(4-Methoxy-benzyl)-3,4-diaza-bicyclo[4.1.0]heptan-2,5-dione

생성물 1

HCID 19936399HCID 19936399, 화합물수율 29.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 5 ml of methylene chloride was added 462 mg (1.87 mmol) of (±)-3-(4-methoxybenzyl)-3,4-diazabicyclo[4.1.0]heptane-2,5-dione obtained in Reference Example 19. The mixture was cooled on a dry ice/ethanol bath, and 0.1 ml (1.1 mmol) of boron tribromide was added thereto dropwise. The temperature was elevated to room temperature, and the mixture was stirred for 2 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, the solvent was removed by distillation under reduced pressure, and the residue was recrystallized from ethanol/chloroform to obtain 120 mg (29.6%) of the titled compound.

후처리

  1. customobtained in Reference Example 19
  2. temperatureThe mixture was cooled on a dry ice/ethanol bath
  3. customwas elevated to room temperature
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customthe solvent was removed by distillation under reduced pressure
  7. customthe residue was recrystallized from ethanol/chloroform

출처 및 근거

ORD 기록
ord-2154e15dceea4bc7b34faa003c458041
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05418232

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