Benzyl Bromide → HCID 12827154、化合物

HRID 1485836ノート

反応式

HRID 1485836 の反応式
[CH:1]1([OH:8])[CH2:6][CH2:5][CH:4]([OH:7])[CH:3]=[CH:2]1.[H-].[Na+].[CH2:11](Br)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>CN(C=O)C>[CH2:11]([O:7][CH:4]1[CH2:5][CH2:6][CH:1]([OH:8])[CH:2]=[CH:3]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 5508252-Cyclohexene-1,4-diol

生成物 1

HCID 12827154HCID 12827154、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 34 (79 mg, 0.69 mmol) in DMF (1 mL) was added sodium hydride (14 mg, 0.62 mmol) at 0° C. Benzyl bromide (73 μL, 0.62 mmol) was added to the mixture dropwise, under an argon atmosphere. The reaction was stirred for 16 h at room temperature. Upon completion, distilled water (3 mL) was added to the mixture and the organic layer extracted into ethyl acetate. The organic layers were combined, dried and concentrated to give a crude mixture that was purified by column chromatography (Silica gel, 10%-20% EtOAc in hexane) to give 35 as an oil.

後処理

  1. distillationUpon completion, distilled water (3 mL)
  2. additionwas added to the mixture
  3. extractionthe organic layer extracted into ethyl acetate
  4. customdried
  5. concentrationconcentrated
  6. customto give a crude mixture that
  7. customwas purified by column chromatography (Silica gel, 10%-20% EtOAc in hexane)

出典と根拠

ORDレコード
ord-ec927e1369724cf0bc30af60a8959100
出典データセット
uspto-grants-2016_08
特許番号
US09422320B2

反応ノート

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