Hexane → HCID 178419089, 화합물

HRID 273975

반응식

HRID 273975 반응식
CCCCCC.C([Li:11])CCC.CC(C)([O-])C.[K+].[F:18][C:19]1[C:20]([F:28])=[C:21]([F:27])[C:22]([F:26])=[C:23]([F:25])[CH:24]=1>C(OCC)C>[F:18][C:19]1[C:24]([Li:11])=[C:23]([F:25])[C:22]([F:26])=[C:21]([F:27])[C:20]=1[F:28]

참가 물질

6

반응물 4

HCID 8058HexaneHCID 9696PentafluorobenzeneHCID 23665647Potassium tert-butoxideHCID 178418339Butyllithium

생성물 1

HCID 178419089HCID 178419089, 화합물수율 95.9%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
-65 °C

실험 절차

Inside of a 100 ml volume glass three-neck flask equipped with a 50 ml volume glass dropping funnel, temperature resistor and septum rubber was sufficiently replaced with nitrogen. Into the flask, 15.5 g (29.8 mmol) hexane solution of 15.5 wt. % butyllithium, 3.3 g (29.8 mmol) potassium tertbutoxide and 15 ml diethyl ether were charged, of which solution was cooled to -65° C. Thereafter, 5 g (29.8 mmol) pentafluorobenzene and 15 ml diethyl ether charged into the dropping funnel were added dropwise while making the inner temperature not to exceed -55° C. After the completion of dropwise addition, the reaction mixture was kept at a temperature of -65°~-55° C. with stirring to give pentafluorophenyllithium.

후처리

  1. customInside of a 100 ml volume glass three-neck flask equipped with a 50 ml volume glass
  2. additionwere added dropwise
  3. customto exceed -55° C
  4. additionAfter the completion of dropwise addition
  5. customwas kept at a temperature of -65°~-55° C.

출처 및 근거

ORD 기록
ord-00d91504ec0d41dcb5d1611297681646
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387727

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