3-Chloro-5-(trifluoromethyl)picolinaldehyde oxime → 3-Chloro-5-(trifluoromethyl)pyridine-2-carbonitrile

HRID 340216

反応式

HRID 340216 の反応式
[Cl:1][C:2]1[C:3]([CH:12]=[N:13]O)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.CC[N+](S(N=C(OC)[O-])(=O)=O)(CC)CC>O1CCCC1.C(OCC)(=O)C.O>[Cl:1][C:2]1[C:3]([C:12]#[N:13])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:9])[F:10])[CH:7]=1

参加物

6

反応物 2

HCID 7182493-Chloro-5-(trifluoromethyl)picolinaldehyde oximeHCID 2724994Methyl N-(triethylammoniosulfonyl)carbamate

生成物 1

HCID 14733743-Chloro-5-(trifluoromethyl)pyridine-2-carbonitrile

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 3-chloro-5-(trifluoromethyl)picolinaldehyde oxime (1.0 eq.) and Burgess reagent (1.5 eq.) in tetrahydrofuran (0.5 M) was heated to 65° C. and stirred for 1 hour. The reaction was cooled to room temperature and diluted with ethyl acetate and water. The organic layer was washed with water, brine, dried over anhydrous MgSO4, and concentrated en vacuo to give a solid that was carried onto the next step without further purification.

後処理

  1. washThe organic layer was washed with water, brine
  2. dry with materialdried over anhydrous MgSO4
  3. concentrationconcentrated en vacuo
  4. customto give a solid
  5. customthat was carried onto the next step without further purification

出典と根拠

ORDレコード
ord-60b799d726c742ca8d4da0ea1566b81f
出典データセット
uspto-grants-2014_11
特許番号
US08895577B2

関連ノート

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