Sodium Carbonate → Hexaethyldisiloxane

HRID 1088032ノート

反応式

HRID 1088032 の反応式
C([O:4][Si:5]([CH2:10][CH3:11])([CH2:8][CH3:9])[CH2:6][CH3:7])(=O)C.S[C:13]1[CH:18]=CN=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>>[CH2:6]([Si:5]([O:4][Si:5]([CH2:6][CH3:7])([CH2:8][CH3:9])[CH2:10][CH3:11])([CH2:18][CH3:13])[CH2:8][CH3:9])[CH3:7]

参加物

4

反応物 3

HCID 10340Sodium CarbonateHCID 79173Silanol, 1,1,1-triethyl-, 1-acetateHCID 178418431pyridine-4-thiol

生成物 1

HCID 70442Hexaethyldisiloxane収率 71%

実験手順

This solution of chloride (4) is mixed with 4-mercaptopyridine (2.45 g; 1.3 equivalents) and sodium carbonate (1.8 g; 1 equivalents) and concentrated in vacuum. The residue is dissolved in toluene, filtered to remove solid, and extracted with toluene. This is extracted with 2N-hydrochloric acid, mixed with sodium hydrogen carbonate, reextracted with toluene, and worked up as usual to give 4-pyridylsulfide (7) (7.87 g). Yield: 71%. IR (CHCl3)ν: 3100-2900, 1735, 1707, 1610, 1430 cm-1.

後処理

  1. concentrationconcentrated in vacuum
  2. dissolutionThe residue is dissolved in toluene
  3. filtrationfiltered
  4. customto remove solid
  5. extractionextracted with toluene
  6. extractionThis is extracted with 2N-hydrochloric acid
  7. additionmixed with sodium hydrogen carbonate

出典と根拠

ORDレコード
ord-d1c4f8a9f51744e99b7fe505f9a76c08
出典データセット
uspto-grants-1990_10
特許番号
US04960879

反応ノート

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