Hydrochloric Acid → 2-Chloro-3-fluoro-benzamidine

HRID 1804540ノート

反応式

HRID 1804540 の反応式
C[Si](C)(C)[N-:3][Si](C)(C)C.[Li+].[Cl:11][C:12]1[C:19]([F:20])=[CH:18][CH:17]=[CH:16][C:13]=1[C:14]#[N:15].Cl>CCCCCC.C(OCC)C>[Cl:11][C:12]1[C:19]([F:20])=[CH:18][CH:17]=[CH:16][C:13]=1[C:14]([NH2:3])=[NH:15]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 2733832Lithium HexamethyldisilazideHCID 37235862-Chloro-3-fluorobenzonitrile

生成物 1

HCID 576985762-Chloro-3-fluoro-benzamidine

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒

実験手順

320 ml (0.32 mmol) of a 1 molar solution of lithium hexamethyl disilazide (LiHMDS) in hexane are placed in 800 ml diethyl ether and combined at ambient temperature with 25.0 g (0.161) 2-chloro-3-fluoro-benzonitrile. The mixture is stirred for 2 h at ambient temperature and after cooling to 0° C. it is combined with 280 ml 3 normal hydrochloric acid. The precipitate formed is suction filtered, washed with water and dried.

後処理

  1. temperatureafter cooling to 0° C. it
  2. customThe precipitate formed
  3. filtrationfiltered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-8c300e53f2994e4a8d7fa6c0ef48ca95
出典データセット
uspto-grants-2013_01
特許番号
US08354418B2

反応ノート

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