4-Bromo-3,3,4,4-tetrafluorobutan-1-ol → 4-Hydroxy-1,1,2,2-tetrafluorobutane-1-sulfonic acid

HRID 1395955ノート

反応式

HRID 1395955 の反応式
[OH:1][CH2:2][CH2:3][C:4]([F:13])([F:12])[C:5]([F:11])([F:10])[S:6]([O-:9])(=[O:8])=[O:7].[Na+].BrC(F)(F)C(F)(F)CCO>CO>[OH:1][CH2:2][CH2:3][C:4]([F:13])([F:12])[C:5]([F:10])([F:11])[S:6]([OH:9])(=[O:7])=[O:8]

参加物

4

反応物 2

HCID 27363694-Bromo-3,3,4,4-tetrafluorobutan-1-olHCID 58463092Sodium 1,1,2,2-tetrafluoro-4-hydroxybutane-1-sulfonate

生成物 1

HCID 584630934-Hydroxy-1,1,2,2-tetrafluorobutane-1-sulfonic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The solid from above which contained sodium 4-hydroxy-1,1,2,2-tetrafluorobutane-1-sulfonate was extracted with methanol (100 mL) and filtered. The resulting pale yellow solution was passed through a short column (2.5 cm diameter) which was packed with 7.5 cm of Amberlite 120H acid ion exchange resin to give a light brown solution. Additional methanol was used to flush any remaining sulfonic acid. The volatiles were removed under reduced pressure to give a dark brown oil. The yield was 15.453 g, 77% based on starting 4-bromo-3,3,4,4-tetrafluoro-1-butanol.

後処理

  1. extractionwas extracted with methanol (100 mL)
  2. filtrationfiltered
  3. customto give a light brown solution
  4. customto flush any remaining sulfonic acid
  5. customThe volatiles were removed under reduced pressure
  6. customto give a dark brown oil

出典と根拠

ORDレコード
ord-abef295c47084e70a76e02e0c35b889b
出典データセット
uspto-grants-2014_12
特許番号
US08900792B2

反応ノート

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