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HCID 4232364、化合物 → 4,4-Dimethyl-4-silapentane-1-sulfonic acid

HRID 2184068
ノート
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反応式

HRID 2184068 の反応式
[CH3:1][Si:2]([CH3:11])([CH3:10])[CH2:3][CH2:4][CH2:5][S:6]([O-:9])(=[O:8])=[O:7].[Na+].C[Si](C)(C)CCCS([O-])(=O)=O>O>[CH3:10][Si:2]([CH3:1])([CH3:11])[CH2:3][CH2:4][CH2:5][S:6]([OH:9])(=[O:8])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4232364HCID 4232364、化合物HCID 5167273Sodium 3-(trimethylsilyl)-1-propanesulfonate

生成物 1

HCID 748734,4-Dimethyl-4-silapentane-1-sulfonic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of sodium 3-(trimethylsilyl)-1-propanesulfonate (9 grams, 41.2 mmol) dissolved in demineralized water (75 ml) was added drop wise into a short column packed with an excess (15-20 times the molar amount of 3-(trimethylsilyl)-1-propanesulfonate) of Tulsion T-42 MP(H+) acidic ion exchange resin. Then the resin bed was washed with water until the pH of the solution eluting from the column was about 5 to 6. The water solution of the free 3-(trimethylsilyl)-1-propanesulfonic acid thus obtained was neutralized with tetra-n-butylammonium hydroxide until the pH of the solution was about 5 to 5.5. The resulting mixture was extracted with chloroform (three times) and the combined chloroform washes was washed with water (three times). The chloroform layer was separated, dried with anhydrous sodium sulfate, and concentrated under reduced pressure to remove solvent and other volatiles. The residual material was finally dried at 40° C. and 0.1 mm Hg to afford tetra-n-butylammonium 3-(trimethylsilyl)-1-propanesulfonate as a hygroscopic white solid. The yield of the product was 17.4 grams, or 97% of the theoretical amount. Proton NMR spectrum of the compound indicated that it was the desired compound.

後処理

  1. additionwas added drop wise into a short column
  2. washThen the resin bed was washed with water until the pH of the solution
  3. washeluting from the column

出典と根拠

ORDレコード
ord-5c247059d4f94d9aabee178391990264
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06900257B2

反応ノート

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