Benzaldehyde → HCID 14801250、化合物

HRID 985754ノート

反応式

HRID 985754 の反応式
[CH:1]([F:10])([F:9])[C:2]([F:8])([F:7])[C:3]([F:6])([F:5])[F:4].[Li][C:12]([CH3:15])([CH3:14])C.[CH:16](=[O:23])[C:17]1C=CC=C[CH:18]=1.Cl>CCCCC.CCOCC>[F:7][C:2]([F:8])([C:3]([F:6])([F:5])[F:4])[C:1]([C:14]1[CH:12]=[CH:15][CH:18]=[CH:17][C:16]=1[OH:23])([F:10])[F:9]

参加物

7

反応物 4

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 624421H-PerfluoropropaneHCID 178418306HCID 178418306、化合物

生成物 1

HCID 14801250HCID 14801250、化合物収率 70%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8003Pentane溶媒

反応条件

温度
-80 °C

実験手順

60 ml of ether and 3.6 g (30 mmol) of 1H-heptafluoropropane were placed in a 4-neck flask fitted with anchor stirrer, dropping funnel, and internal thermometer and the mixture was cooled to −80° C. 9 g (20 mmol) of tert-BuLi as a 15% strength solution in pentane were then added dropwise and the mixture was stirred for another 30 minutes at this temperature. 2.1 g (20 mmol) of benzaldehyde in 10 ml of ether were subsequently added dropwise. After stirring at −80° C. for 2 hours, the yellow solution was allowed to come to room temperature and dilute hydrochloric acid was added. The mixture was extracted three times with ether and the combined organic phases were dried and filtered. Purification by distillation gave heptafluoropropylphenyl alcohol in a yield of 70%.

後処理

  1. customfitted with anchor stirrer
  2. stirringAfter stirring at −80° C. for 2 hours
  3. customto come to room temperature
  4. extractionThe mixture was extracted three times with ether
  5. customthe combined organic phases were dried
  6. filtrationfiltered
  7. customPurification
  8. distillationby distillation

出典と根拠

ORDレコード
ord-9c7e8110ac8c4e01a719cf02ac99a3d9
出典データセット
uspto-grants-2005_03
特許番号
US06872861B2

反応ノート

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