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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethyl Acetate → 4-(2,3-Dihydro[1,4]benzodioxin-5-yl)pyridine

HRID 1107423
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인쇄 미리보기

반응식

HRID 1107423 반응식
C(B(CC)[C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)C.Br[C:13]1[C:22]2[O:21][CH2:20][CH2:19][O:18][C:17]=2[CH:16]=[CH:15][CH:14]=1.[OH-].[K+].C(OCC)(=O)C>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[O:18]1[C:17]2[CH:16]=[CH:15][CH:14]=[C:13]([C:4]3[CH:5]=[CH:6][N:7]=[CH:8][CH:9]=3)[C:22]=2[O:21][CH2:20][CH2:19]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 14797Potassium HydroxideHCID 133188714-(Diethylboranyl)pyridineHCID 187872685-Bromo-2,3-dihydro-1,4-benzodioxine

생성물 1

HCID 109327794-(2,3-Dihydro[1,4]benzodioxin-5-yl)pyridine

시약·촉매·용매 3

HCID 74236Tetrabutylammonium Bromide
촉매
HCID 178418397HCID 178418397, 화합물촉매
HCID 8028Tetrahydrofuran용매

실험 절차

14.7 mmol of diethyl(pyrid-4-yl)borane, 22 mmol of 5-bromo-2,3-dihydro[1,4]benzodioxine, 44.1 mol of KOH in powder form, 7.4 mmol of tetrabutylammonium bromide and 0.74 mmol of tetrakis(triphenylphosphine)palladium in 75 ml of tetrahydrofuran are mixed at room temperature, and the mixture is then refluxed for 24 hours. 225 ml of ethyl acetate are added and the mixture is washed with a saturated sodium chloride solution. Drying is carried out over MgSO4, followed by evaporation and purification over a silica column (eluant CH2Cl2,then CH2Cl2 /CH3COOC2H5 80/20).

후처리

  1. temperaturethe mixture is then refluxed for 24 hours
  2. washthe mixture is washed with a saturated sodium chloride solution
  3. customDrying
  4. customfollowed by evaporation and purification over a silica column (eluant CH2Cl2,then CH2Cl2 /CH3COOC2H5 80/20)

출처 및 근거

ORD 기록
ord-e224160d476246a6bfdd1a028b1594ab
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06060487

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