Diethyl Ether → HCID 57445526、化合物

HRID 2238604ノート

反応式

HRID 2238604 の反応式
C1C=C[NH+]=CC=1.[O-][Cr](Cl)(=O)=O.[C:12]1([CH2:18][CH2:19][CH:20]2[C:24]3[CH:25]=[C:26]([CH2:29][OH:30])[CH:27]=[CH:28][C:23]=3[O:22][CH2:21]2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(OCC)C>C(Cl)Cl>[C:12]1([CH2:18][CH2:19][CH:20]2[C:24]3[CH:25]=[C:26]([CH:29]=[O:30])[CH:27]=[CH:28][C:23]=3[O:22][CH2:21]2)[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 23081965HCID 23081965、化合物HCID 178418287HCID 178418287、化合物

生成物 1

HCID 57445526HCID 57445526、化合物収率 67%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of PCC (3.69 g, 17.10 mmol) in methylene chloride (20 ml), a solution of 3-(2-phenylethyl)-2,3-dihydro-1-benzofuran-5-yl-methanol (3.32 g, 13.16 mmol) in methylene chloride (100 ml) was added at room temperature. After stirring for 12 h, diethyl ether (300 ml) was added and the black solid precipitated was filtered and washed with diethyl ether several times. The filtrate was concentrated under vacuum and the residue was purified by flash chromatography on silica gel (petroleum ether/ethyl acetate=95/5-9/1) affording 0.202 g of the title compound (67% yield).

後処理

  1. customthe black solid precipitated
  2. filtrationwas filtered
  3. washwashed with diethyl ether several times
  4. concentrationThe filtrate was concentrated under vacuum
  5. customthe residue was purified by flash chromatography on silica gel (petroleum ether/ethyl acetate=95/5-9/1)

出典と根拠

ORDレコード
ord-3f71a010d1104ea2beb9844d82768eb3
出典データセット
uspto-grants-2010_05
特許番号
US07718815B2

反応ノート

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