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Dichloromethane → HCID 22226103, 화합물

HRID 1744911
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HRID 1744911 반응식
[C:1](Cl)(=[O:3])[CH3:2].[CH2:5]([O:8][C:9]1[CH:10]=[CH:11][C:12]2[C:13]([CH3:22])([CH3:21])[CH2:14][CH2:15][C:16]([CH3:20])([CH3:19])[C:17]=2[CH:18]=1)[CH2:6][CH3:7].[Cl-].[Cl-].[Cl-].[Al+3].Cl[CH2:28]Cl>>[CH2:5]([O:8][C:9]1[C:10]([C:1](=[O:3])[CH2:2][CH3:28])=[CH:11][C:12]2[C:13]([CH3:21])([CH3:22])[CH2:14][CH2:15][C:16]([CH3:20])([CH3:19])[C:17]=2[CH:18]=1)[CH2:6][CH3:7]
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5

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HCID 6344DichloromethaneHCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 222261103-n-Propoxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalene2회

생성물 1

HCID 22226103HCID 22226103, 화합물

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온도
0 °C

실험 절차

Acetyl chloride (0.831 g, 11.7 mmol) was added to a stirring solution of 3-n-propoxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalene (Intermediate 6, 2.4 g, 9.7 mmol) in dichloromethane (100 mL), and the solution was cooled to 0° C. Aluminum trichloride (1.56 g, 11.7 mmol) was added over two to three minutes, the ice-bath was removed, the yellow solution was stirred for 1 h at room temperature. The solution was poured over ice in a separatory funnel, and the products were extracted three times with ether. The combined organic layers were washed with 10% aqueous sodium hydroxide, brine and dried over magnesium sulfate. The solvent was removed in vacuo to give the title compound as a solid.

후처리

  1. customthe ice-bath was removed
  2. additionThe solution was poured over ice in a separatory funnel
  3. extractionthe products were extracted three times with ether
  4. washThe combined organic layers were washed with 10% aqueous sodium hydroxide, brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-9b119ade55ee4eddb885dd59d670fbab
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07019034B2

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