Potassium bisulfate → 4-{[tert-Butyl(dimethyl)silyl]oxy}butanoic acid

HRID 514464ノート

反応式

HRID 514464 の反応式
[Si:1]([O:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][Li])=[O:13])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].OS([O-])(=O)=O.[K+]>C(OCC)(=O)C>[Si:1]([O:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 516920Potassium bisulfateHCID 178506949HCID 178506949、化合物

生成物 1

HCID 1868234-{[tert-Butyl(dimethyl)silyl]oxy}butanoic acid収率 95%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-[tert-butyl(dimethyl)silyl]oxybutanoyloxylithium (8.0 g, 35.71 mmol) in ethyl acetate (10 mL), was carefully added KHSO4 (5%) to adjust pH to about 1. It was then extracted with ethyl acetate three times and organic extracts washed with brine and dried with anhydrous NaSO4. The organic extracts were concentrated to give the title compound (7.4 g, 95%). [M+H] Calc'd for C10H22O3Si, 219. Found, 219.

後処理

  1. extractionIt was then extracted with ethyl acetate three times and organic extracts
  2. washwashed with brine
  3. dry with materialdried with anhydrous NaSO4
  4. concentrationThe organic extracts were concentrated

出典と根拠

ORDレコード
ord-f5a605304d5f458eaca8a8ebc79e3d17
出典データセット
uspto-grants-2015_08
特許番号
US09107916B2

反応ノート

読み込み中…