1,3-Difluoro-2-propanol → 3-(2-Fluoro-1-fluoromethyl-ethoxy)-4-nitro-benzonitrile

HRID 532273ノート

反応式

HRID 532273 の反応式
[F:1][CH2:2][CH:3]([OH:6])[CH2:4][F:5].[Li+].C[Si]([N-][Si](C)(C)C)(C)C.F[C:18]1[CH:19]=[C:20]([CH:23]=[CH:24][C:25]=1[N+:26]([O-:28])=[O:27])[C:21]#[N:22]>C1COCC1.O>[F:1][CH2:2][CH:3]([CH2:4][F:5])[O:6][C:24]1[CH:23]=[C:20]([CH:19]=[CH:18][C:25]=1[N+:26]([O-:28])=[O:27])[C:21]#[N:22]

参加物

6

反応物 3

HCID 679851,3-Difluoro-2-propanolHCID 2733832Lithium HexamethyldisilazideHCID 27833993-Fluoro-4-nitrobenzonitrile

生成物 1

HCID 584133843-(2-Fluoro-1-fluoromethyl-ethoxy)-4-nitro-benzonitrile

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

1,3-Difluoro-propan-2-ol (4.2 g) was dissolved under argon in THF (250 ml) and cooled to 0° C. LiHMDS (28 ml) was added to the mixture and stirred at rt for 1 hour. Then the mixture was cooled to 0° C. and 3-fluoro-4-nitrobenzonitrile (1.95 ml) was added in portions and stirred for 2 hours. The mixture was poured in water and extracted with DCM. The organic layer was washed with water, dried and concentrated.

後処理

  1. temperatureThen the mixture was cooled to 0° C.
  2. stirringstirred for 2 hours
  3. extractionextracted with DCM
  4. washThe organic layer was washed with water
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-4b72932b3cb84c42ac26ae000d7ed6bb
出典データセット
uspto-grants-2014_10
特許番号
US08853193B2

反応ノート

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