Triethylamine → 9-Methoxymethyl-9-triethylsilyloxymethyl-fluorene

HRID 2416164ノート

反応式

HRID 2416164 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.[CH2:26]([Si:28](Cl)([CH2:31][CH3:32])[CH2:29][CH3:30])[CH3:27]>ClCCl>[CH3:1][O:2][CH2:3][C:4]1([CH2:17][O:18][Si:28]([CH2:31][CH3:32])([CH2:29][CH3:30])[CH2:26][CH3:27])[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 8471TriethylamineHCID 13819ChlorotriethylsilaneHCID 226391039-(Methoxymethyl)-9H-fluorene-9-methanol

生成物 1

HCID 226390909-Methoxymethyl-9-triethylsilyloxymethyl-fluorene収率 84%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1 g of 9-methoxymethyl-9-hydroxymethyl-fluorene (4.2 mmol) was dissolved in 20 ml of dichloromethane. The solution was cooled in ice-water bath, and 0.87 ml of triethyl amine (6.2 mmol) was added thereto. After stirring for 5 minutes, 0.91 ml of triethylsilyl chloride (5.4 mmol) 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 1.24 g of concentrate (yield 84%).

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 1.24 g
  9. concentrationof concentrate (yield 84%)

出典と根拠

ORDレコード
ord-7375db9db7c94fd999b11389e37dc825
出典データセット
uspto-grants-2004_11
特許番号
US06822109B2

反応ノート

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