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Triethylamine → 1-Phthalimido-4-p-toluenesulfonyl-6,6-difluoro-8-hydroxy-4-aza-octane

HRID 2072888
ノート
印刷プレビュー

反応式

HRID 2072888 の反応式
[C:1]1(=[O:39])[N:5]([CH2:6][CH2:7][CH2:8][N:9]([S:24]([C:27]2[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][CH:28]=2)(=[O:26])=[O:25])[CH2:10][C:11]([F:23])([F:22])[CH2:12][CH2:13][O:14]CC2C=CC=CC=2)[C:4](=[O:34])[C:3]2=[CH:35][CH:36]=[CH:37][CH:38]=[C:2]12.C[Si](I)(C)C.C(N(CC)CC)C>ClCCl.CO>[C:4]1(=[O:34])[N:5]([CH2:6][CH2:7][CH2:8][N:9]([S:24]([C:27]2[CH:28]=[CH:29][C:30]([CH3:33])=[CH:31][CH:32]=2)(=[O:25])=[O:26])[CH2:10][C:11]([F:23])([F:22])[CH2:12][CH2:13][OH:14])[C:1](=[O:39])[C:2]2=[CH:38][CH:37]=[CH:36][CH:35]=[C:3]12
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 85247Trimethylsilyl iodideHCID 198607071-Phthalimido-4-p-toluenesulfonyl-6,6-difluoro-8-benzyloxy-4-aza-octane

生成物 1

HCID 198606861-Phthalimido-4-p-toluenesulfonyl-6,6-difluoro-8-hydroxy-4-aza-octane

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

A solution of 1-phthalimido-4-p-toluenesulfonyl-6,6-difluoro-8-benzyloxy-4-aza-octane (9.5 g, 17.1 mM) and trimethylsilyl iodide (2.7 mL, 10% excess) in dry dichloromethane is stirred overnight at room temperature under nitrogen. Triethylamine (3 g) is added, and stirring is continued for 1 hour at room temperature. Following the addition of more dichloromethane, the reaction mixture is washed with 1N HCL (twice), aqueous NaHSO3 (twice), brine (twice), and dried (Na2SO4). The solvents are removed by evaporation to yield an oil. This oil is dissolved in methanol and 1 mL of a 9N solution of HCL in methanol is added. The mixture is evaporated and stripped twice with CCl4 to provide an oil, which upon scratching with ether/petroleum ether yields 1-phthalimido-4-p-toluenesulfonyl-6,6-difluoro-8-hydroxy-4-aza-octane as slightly violet crystals: 6.8 g (85%).

後処理

  1. washthe reaction mixture is washed with 1N HCL (twice), aqueous NaHSO3 (twice), brine (twice), and
  2. dry with materialdried (Na2SO4)
  3. customThe solvents are removed by evaporation
  4. customto yield an oil
  5. customThe mixture is evaporated
  6. customto provide an oil, which

出典と根拠

ORDレコード
ord-a4f2e3d9d8914736927abd39456c4138
出典データセット
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04914240

反応ノート

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