Hydrochloric Acid → 950-04-9

HRID 2102888ノート

反応式

HRID 2102888 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]#[C:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([O-:11])=[O:10])=[CH:7][CH:6]=1.[OH-].[Li+].CO.Cl>O>[F:1][C:2]([F:14])([F:15])[C:3]#[C:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[CH:7][CH:6]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 3939Lithium HydroxideHCID 86607391HCID 86607391、化合物

生成物 1

HCID 57804103950-04-9収率 87%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a 100 mL round bottom flask was added 4-(3,3,3-trifluoroprop-1-ynyl)benzoate (0.68 g, 2.9 mmol), lithium hydroxide (0.71 g, 29 mmol), and methanol (30 mL): water (10 mL). The mixture was stirred at room temperature for 30 minutes, heated at reflux for 1 hour, and reduced in vacuo. Water (100 mL) was added and the mixture was cooled to 0° C. HCl (10 N) was added slowly to the stirred solution until the pH of the solution reached 5. A yellow precipitate formed and was filtered, washed with cold water (3×100 mL), and dried under vacuum to afford 0.540 g (86%) of 4-(3,3,3-trifluoroprop-1-ynyl)benzoic acid as a light yellow solid.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. temperaturethe mixture was cooled to 0° C
  4. customA yellow precipitate formed
  5. filtrationwas filtered
  6. washwashed with cold water (3×100 mL)
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-62db2978f84d4357bc9f23fb9ae8d31e
出典データセット
uspto-grants-2009_08
特許番号
US07576099B2

反応ノート

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