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Hydrochloric Acid → 2-(1,3-Isoindolinedion-2-yl)-5-(2-methylpropionyl)indane

HRID 1598560
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인쇄 미리보기

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HRID 1598560 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][CH:6]([CH3:10])[C:7](Cl)=[O:8].[C:11]1(=[O:30])[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13](=[O:20])[N:12]1[CH:21]1[CH2:29][C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22]1.Cl>ClC(Cl)C>[C:11]1(=[O:30])[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13](=[O:20])[N:12]1[CH:21]1[CH2:22][C:23]2[C:28](=[CH:27][CH:26]=[C:25]([C:7](=[O:8])[CH:6]([CH3:10])[CH3:5])[CH:24]=2)[CH2:29]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 62325Isobutyryl chlorideHCID 6451240Aluminum(III) ChlorideHCID 109998862-(1,3-Isoindolinedion-2-yl)indane

생성물 1

HCID 189297332-(1,3-Isoindolinedion-2-yl)-5-(2-methylpropionyl)indane수율 73.7%

시약·촉매·용매 1

HCID 6365
1,1-Dichloroethane
용매
2회

실험 절차

To 8.00 g of anhydrous aluminum chloride suspended in 100 ml of dichloroethane was added dropwise 3.20 g of 2-methylpropanoyl chloride dissolved in 50 ml of dichloroethane under ice cooling. Then, to the mixture was added 5.27 g of 2-(1,3-isoindolinedion-2-yl)indane, and the mixture was stirred for 3 hours. The reaction mixture was poured into ice water containing hydrochloric acid, the organic layer was collected by separation, washed with water and dried, and then the solvent was removed. The resulting crystals were recrystallized from ethyl acetate-n-hexane to obtain 4.92 g of 2-(1,3-isoindolinedion-2-yl )-5-(2-methylpropionyl)indane.

후처리

  1. customthe organic layer was collected by separation
  2. washwashed with water
  3. customdried
  4. customthe solvent was removed
  5. customThe resulting crystals were recrystallized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-e98663a244644d49b7c487da4ccbe87f
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05739132

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