Hexane → HCID 12037344、化合物

HRID 1639734ノート

反応式

HRID 1639734 の反応式
[CH2:1]([C:4]1[CH:9]=[C:8]([Br:10])[CH:7]=[CH:6][C:5]=1[OH:11])[CH:2]=[CH2:3].[C:12](=O)([O-])[O-].[K+].[K+].[CH2:18]([O:25][CH:26](Cl)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29]C=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.CCCCCC>CN(C)C=O.C(OCC)(=O)C>[CH2:1]([C:4]1[CH:9]=[C:8]([Br:10])[CH:7]=[CH:6][C:5]=1[O:11][CH2:12][C:31]1[CH:32]=[CH:27][C:26]([O:25][CH2:18][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[CH:29][CH:30]=1)[CH:2]=[CH2:3]

参加物

7

反応物 4

HCID 8058HexaneHCID 11430Potassium CarbonateHCID 2584682-ALLYL-4-BROMOPHENOL2 回HCID 21972261HCID 21972261、化合物

生成物 1

HCID 12037344HCID 12037344、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Under an atmosphere replaced with argon, 2-allyl-4-bromophenol (compound 3), potassium carbonate and benzyloxy-benzylchloride (BnBr) were dissolved in dimethylformamide (DMF), and stirred at room temperature for 3 hours. After confirming that the starting materials were disappeared using thin-layer chromatography (TLC) (with a developer of n-hexane:ethyl acetate=4:1), the reaction liquid was subjected to extraction using 20 mL of water and 20 mL of ethyl acetate. The organic phase was washed with 20 mL of water twice, dried using magnesium sulfate, and then subjected to filtration. The filtrate was concentrated under reduced pressure using an evaporator. The resultant residue was subjected to purification using silica gel flash chromatography (silica gel flash c.c.) (with a developer of n-hexane:ethyl acetate×4:1), to thereby obtain 2-allyl-1-(4-benzyloxy-benzyloxy)-4-bromobenzene (compound 4) as light brown solid.

後処理

  1. extractionwas subjected to extraction
  2. washThe organic phase was washed with 20 mL of water twice
  3. customdried
  4. filtrationsubjected to filtration
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customan evaporator
  7. customThe resultant residue was subjected to purification

出典と根拠

ORDレコード
ord-5782abed08dd4c178da8be4447310698
出典データセット
uspto-grants-2012_02
特許番号
US08110601B2

反応ノート

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