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Methanol → 1,3-Bis(2-hydroxyethylthio)propane

HRID 258786
ノート
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反応式

HRID 258786 の反応式
[Na+].[SH-:2].[SH:3][CH2:4][CH2:5][OH:6].[CH3:7][O-:8].[Na+].Cl[CH2:11][CH2:12][CH2:13]Cl.[CH3:15]O>>[OH:6][CH2:5][CH2:4][S:3][CH2:11][CH2:12][CH2:13][S:2][CH2:15][CH2:7][OH:8]
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 5

HCID 887MethanolHCID 15672-Mercaptoethanol2 回HCID 88811,3-DichloropropaneHCID 28015Sodium hydrosulfideHCID 10942334Sodium Methoxide

生成物 1

HCID 3737351,3-Bis(2-hydroxyethylthio)propane収率 95%

実験手順

The sodium mercaptide of 2-mercaptoethanol was made by reacting 1 mole each of sodium methoxide and 2-mercaptoethanol in dry methanol under a nitrogen atmosphere. To this solution, 0.5 mole of 1,3-dichloropropane was added and the mixture was refluxed for 1 hour and filtered. The methanol filtrate was evaporated on a flash evaporator and traces of 2-mercaptoethanol were distilled off at high vacuum at room temperature. The yellow, oily residue was extracted with acetone, the solution filtered, and the acetone evaporated to give a 95 percent yield of the crude product.

後処理

  1. temperaturethe mixture was refluxed for 1 hour
  2. filtrationfiltered
  3. customThe methanol filtrate was evaporated on a flash evaporator and traces of 2-mercaptoethanol
  4. distillationwere distilled off at high vacuum at room temperature
  5. extractionThe yellow, oily residue was extracted with acetone
  6. filtrationthe solution filtered
  7. customthe acetone evaporated

出典と根拠

ORDレコード
ord-b8a27b8a1a794ffebfedb31a6d6eee9a
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE029305

反応ノート

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