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Hydrochloric Acid → HCID 14098168, 화합물

HRID 569272
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HRID 569272 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]1([CH2:19][CH2:20][C:21](=[O:23])[CH3:22])[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.[OH-].[Na+].Cl>CO>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]12[CH2:19][CH2:20][C:21](=[O:23])[CH:22]=[C:6]1[C:7]1[C:12](=[CH:11][C:10]([O:14][CH3:15])=[C:9]([Cl:16])[C:8]=1[Cl:17])[CH2:13]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 14098167HCID 14098167, 화합물

생성물 1

HCID 14098168HCID 14098168, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-(3-Chloropropyl)-6,7-dichloro-2,3-dihydro-5-methoxy-2-(3-oxobutyl)-1H-inden-1-one (36 g, 0.0053 mole) was dissolved in methanol (4.75 ml) containing 10% aqueous sodium hydroxide (190 ml). Then stirred and refluxed for 3 hours. The solution was cooled, poured into crushed ice, acidified with hydrochloric acid and the solid that separated removed by filtration. The solid washed on the filter with water, dried and recrystallized from a mixture of tetrahydrofuran and ether to give 9a-(3-chloropropyl)-5,6-dichloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one, 15 g, m.p. 183°-185° C.

후처리

  1. temperaturerefluxed for 3 hours
  2. temperatureThe solution was cooled
  3. additionpoured
  4. custominto crushed ice
  5. customthe solid that separated
  6. customremoved by filtration
  7. washThe solid washed on the
  8. filtrationfilter with water
  9. customdried
  10. customrecrystallized from a mixture of tetrahydrofuran and ether

출처 및 근거

ORD 기록
ord-a9e9f82201af40b9941aef0f3e08a75f
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04731470

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