Benzaldehyde → HCID 14801250, 화합물

HRID 985754노트

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HRID 985754 반응식
[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]

참가 물질

7

반응물 4

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 624421H-PerfluoropropaneHCID 178418306HCID 178418306, 화합물

생성물 1

HCID 14801250HCID 14801250, 화합물수율 70%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8003Pentane용매

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온도
-80 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-9c7e8110ac8c4e01a719cf02ac99a3d9
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06872861B2

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