Chlorotrimethylsilane → 1,2-Difluoro-3-trimethylsilylbenzene

HRID 507895

反応式

HRID 507895 の反応式
[Li]CCCC.[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[F:13].[CH3:14][Si:15](Cl)([CH3:17])[CH3:16].C(OC)(C)(C)C>O1CCCC1.O>[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([Si:15]([CH3:17])([CH3:16])[CH3:14])[C:8]=1[F:13]

参加物

7

反応物 4

HCID 6397ChlorotrimethylsilaneHCID 97061,2-DifluorobenzeneHCID 15413tert-Butyl methyl etherHCID 178418339Butyllithium

生成物 1

HCID 108993711,2-Difluoro-3-trimethylsilylbenzene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

625 ml (1 mol) of 1.6 M BuLi are added dropwise at −78° C. to a solution of 114 g (1 mol) of 1,2-difluorobenzene in 1 l of dry tetrahydrofuran. After 1 hour, 140 ml (120 g, 1.1 mol) of trimethylsilyl chloride are slowly added dropwise at −78° C. The mixture is allowed to warm to room temperature overnight, and then 200 ml of methyl tert-butyl ether and 200 ml of water are added. The organic phase is washed with water (2×100 ml) and sat. NaCl (1×100 ml) and dried using magnesium sulfate, and the solvent is removed under reduced pressure. 170 g (91%) of 5 distil over from the residue at from 100 to 102° C./70 mbar.

後処理

  1. washThe organic phase is washed with water (2×100 ml) and sat. NaCl (1×100 ml)
  2. customdried
  3. customthe solvent is removed under reduced pressure
  4. custom170 g (91%) of 5 distil over from the residue at from 100 to 102° C./70 mbar

出典と根拠

ORDレコード
ord-af7f2b882eda46018fad94137b49add8
出典データセット
uspto-grants-2010_08
特許番号
US07786332B2

関連ノート

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