Hexane → HCID 86732218、化合物
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[F:8].C([Li])CCC.CCCCCC.[F:20][CH2:21][C:22](OCC)=[O:23]>C1COCC1>[F:1][C:2]1[C:3]([F:8])=[CH:4][CH:5]=[CH:6][C:7]=1[C:22](=[O:23])[CH2:21][F:20]参加物
6
実験手順
To a cooled (−78° C.) solution of 1,2-difluorobenzene (8.81 mL, 89 mmol) in THF (175 mL) was added dropwise butyllithium solution, 1.6M in hexane (61.5 mL, 98 mmol). After stirred for 2 h, ethyl fluoroacetate (8.64 mL, 89 mmol) ethyl fluoroacetate was added dropwise. The reaction was stirred for 1 h, the reaction was quenched with saturated NH4Cl and then warmed to room temperature. The resulted mixture was extracted with EtOAc. The organic extracts were washed with brine, dried over Na2SO4 and filtered. The filtrate was concentrated and purified by silica gel column (0-30% EtOAc/hexane) to afford 6.3 g of desired product as colorless oil.
後処理
- stirringThe reaction was stirred for 1 h
- customthe reaction was quenched with saturated NH4Cl
- extractionThe resulted mixture was extracted with EtOAc
- washThe organic extracts were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationThe filtrate was concentrated
- custompurified by silica gel column (0-30% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-9212a8e4f02a4fcabb651f686eb4ea5a
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296734B2
反応ノート
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