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Formaldehyde → HCID 19936097, 화합물

HRID 37633
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HRID 37633 반응식
[Mg].[CH3:2][C:3]([C:6]1[CH:11]=[C:10]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:9]=[CH:8][C:7]=1Br)([CH3:5])[CH3:4].[CH2:17]=[O:18]>O1CCCC1>[CH3:2][C:3]([C:6]1[CH:11]=[C:10]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:9]=[CH:8][C:7]=1[CH2:17][OH:18])([CH3:5])[CH3:4]
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참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 5462224MagnesiumHCID 110764641-Bromo-2,4-di-tert-butylbenzene

생성물 1

HCID 19936097HCID 19936097, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To 243 mg (10 mmoles) of magnesium turnings in 10 ml of tetrahydrofuran is added dropwise a solution of 2.69 grams (10 mmoles) of the title product of Example 9 in 5 ml of tetrahydrofuran. After the addition is complete, the mixture is refluxed for one hour. Paraformaldehyde (1.0 g, excess) is then added, and refluxing continued for one hour. The mixture is cooled to room temperature and partitioned between saturated ammonium chloride and diethyl ether. The aqueous layer is further extracted with ether, the combined organic extracts washed with brine, dried over sodium sulfate, filtered, and evaporated. Chromatography of the residue over silica gel using mixtures of ethyl acetate and hexane as eluents gives the title compound.

후처리

  1. additionAfter the addition
  2. temperaturethe mixture is refluxed for one hour
  3. temperaturerefluxing
  4. custompartitioned between saturated ammonium chloride and diethyl ether
  5. extractionThe aqueous layer is further extracted with ether
  6. washthe combined organic extracts washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated

출처 및 근거

ORD 기록
ord-eef34c5f8cd044d2bf9b0083ff195b7c
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05420343

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