Chlorotrimethylsilane → 9-Methoxymethyl-9-trimethylsilyloxymethyl-fluorene

HRID 2252526ノート

反応式

HRID 2252526 の反応式
[CH3:1][O:2][CH2:3][C:4]1([CH2:17][OH:18])[C:16]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2.C(N(CC)CC)C.[CH3:26][Si:27](Cl)([CH3:29])[CH3:28]>ClCCl>[CH3:1][O:2][CH2:3][C:4]1([CH2:17][O:18][Si:27]([CH3:29])([CH3:28])[CH3:26])[C:16]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2

参加物

5

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 226391039-(Methoxymethyl)-9H-fluorene-9-methanol

生成物 1

HCID 226391279-Methoxymethyl-9-trimethylsilyloxymethyl-fluorene収率 86%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1 g of 9-methoxymethyl-9-hydroxymethyl-fluorene was dissolved in 20 ml of dichloromethane. The solution was cooled in ice-water bath to below 5° C., and 0.7 ml of triethyl amine was added thereto. After stirring for 5 minutes, 0.6 ml of trimethylsilyl chloride was added drop-wise, and the mixture was stirred for further 2 hours, followed by stirring at room temperature for 1 hour. The reaction mixture was washed with water, and the organic layer separated was dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated to give 1.41 g of concentrate (yield 86%). MS(EI) m/e: 312(M+).

後処理

  1. stirringthe mixture was stirred for further 2 hours
  2. stirringby stirring at room temperature for 1 hour
  3. washThe reaction mixture was washed with water
  4. customthe organic layer separated
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. filtrationAfter filtration
  7. customthe filtrate was evaporated
  8. customto give 1.41 g
  9. concentrationof concentrate (yield 86%)

出典と根拠

ORDレコード
ord-93a839d053b8484b942339ec9b198c59
出典データセット
uspto-grants-2008_01
特許番号
US07323431B2

反応ノート

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