Hydrogen Bromide → 12-Bromododecanoic Acid

HRID 1618813

反応式

HRID 1618813 の反応式
[C:1]1(=[O:14])[O:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[BrH:15]>>[Br:15][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][C:1]([OH:13])=[O:14]

参加物

3

反応物 2

HCID 260Hydrogen BromideHCID 70354Oxacyclotridecan-2-one

生成物 1

HCID 17546812-Bromododecanoic Acid収率 86%

実験手順

11.9 g (60.0 mmol) of 12-dodecanolide and 24.3 g (96.0 mmol, 1.6 equivalents) of a 32% (hydrogen bromide)/(acetic acid) solution were introduced into a 100-mL autoclave protected with Teflon (registered trademark), and the autoclave was purged with nitrogen and then sealed. The content in the autoclave was stirred with a magnetic stirrer for 16 hours by using an oil bath at 60° C. After cooling the mixture, 14 mL of water was added thereto, and the mixture was transferred into a separatory funnel by using 200 mL of hot hexane. The mixture was washed with ion-exchanged water, dried over magnesium sulfate, filtered, and crystallized from n-hexane. Thus, 14.4 g (yield: 86%) of 12-bromododecanoic acid was obtained.

後処理

  1. customthe autoclave was purged with nitrogen
  2. customsealed
  3. customat 60° C
  4. temperatureAfter cooling the mixture, 14 mL of water
  5. additionwas added
  6. customthe mixture was transferred into a separatory funnel
  7. washThe mixture was washed with ion-exchanged water
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltered
  10. customcrystallized from n-hexane

出典と根拠

ORDレコード
ord-4361df33b1814b94943413e26b54a429
出典データセット
uspto-grants-2014_07
特許番号
US08771660B2

関連ノート

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