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Water → HCID 14098167, 화합물

HRID 569271
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HRID 569271 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH:5]1[CH2:13][C:12]2[C:7](=[C:8]([Cl:17])[C:9]([Cl:16])=[C:10]([O:14][CH3:15])[CH:11]=2)[C:6]1=[O:18].N12CCCC1=NCCC2.[CH:28]([C:30]([CH3:32])=[O:31])=[CH2:29].O>O1CCCC1>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]1([CH2:29][CH2:28][C:30](=[O:31])[CH3:32])[CH2:13][C:12]2[C:7](=[C:8]([Cl:17])[C:9]([Cl:16])=[C:10]([O:14][CH3:15])[CH:11]=2)[C:6]1=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

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반응물 4

HCID 962WaterHCID 6570Methyl vinyl ketoneHCID 763491,5-Diazabicyclo(4.3.0)non-5-eneHCID 14098166HCID 14098166, 화합물

생성물 1

HCID 14098167HCID 14098167, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2-(3-Chloropropyl)-6,7-dichloro-2,3-dihydro-5-methoxy-1H-inden-1-one (59 g, 0.20 mole) was dissolved in tetrahydrofuran (50 ml) and 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) (3 ml) added. The mixture was stirred and methyl vinyl ketone (28.3 g, 0.404 mole) added dropwise over 30 minutes. The temperature rose from 22° C. to 35° C. over the addition period. The mixture was stirred for an additional hour at ambient temperature, then poured into cold water. The solid that separated was removed by filtration, washed with water, dried and recrystallized from a mixture of tetrahydrofuran and ether to give 2-(3-chloropropyl)-6,7-dichloro-2,3-dihydro-5-methoxy-2-(3-oxobutyl)-1H-inden-1-one, 58.5 g, m.p. 120°-122° C.

후처리

  1. additionThe temperature rose from 22° C. to 35° C. over the addition period
  2. stirringThe mixture was stirred for an additional hour at ambient temperature
  3. customThe solid that separated
  4. customwas removed by filtration
  5. washwashed with water
  6. customdried
  7. customrecrystallized from a mixture of tetrahydrofuran and ether

출처 및 근거

ORD 기록
ord-329d619c6c1e40fbb6ce94397a5d5cff
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04731470

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