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Acetic Acid → HCID 14726499, 화합물

HRID 1728470
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HRID 1728470 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11](=[O:28])[C:12]([C:14]2[CH:23]=[CH:22][C:21]3[C:20]([CH3:25])([CH3:24])[CH2:19][CH2:18][C:17]([CH3:27])([CH3:26])[C:16]=3[CH:15]=2)=[O:13])=[CH:7][CH:6]=1)([O:3]C)=[O:2].C(O)(=O)C.O>S(=O)(=O)(O)O>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11](=[O:28])[C:12]([C:14]2[CH:23]=[CH:22][C:21]3[C:20]([CH3:24])([CH3:25])[CH2:19][CH2:18][C:17]([CH3:27])([CH3:26])[C:16]=3[CH:15]=2)=[O:13])=[CH:7][CH:6]=1)([OH:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 962Water2회HCID 14726493HCID 14726493, 화합물

생성물 1

HCID 14726499HCID 14726499, 화합물수율 85.1%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

3.9 g (10 mmol) of 1-(4-Carbomethoxyphenyl)-2-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)ethanedione (Example 6) were refluxed in a mixture of 5 ml of concentrated sulfuric acid, 80 ml of glacial acetic acid and 40 ml of water for 8 h. The mixture was then poured into 500 ml of water, and the crystalline precipitate was filtered off with suction and washed with water until the washings were neutral. The dried crude product was recrystallized from cyclohexane, yielding 3.1 g of the title compound of melting point 148°-151° C.

후처리

  1. filtrationthe crystalline precipitate was filtered off with suction
  2. washwashed with water until the washings
  3. customThe dried crude product
  4. customwas recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-49d30f68fd2c41de8901b9df63726e28
출처 데이터셋
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05326900

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