Carbon Dioxide → 3-Cyano-2,4-dichlorobenzoic acid

HRID 1288728

反応式

HRID 1288728 の反応式
C([N-]C(C)C)(C)C.[Li+].[Cl:9][C:10]1[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[C:11]=1[C:12]#[N:13].[C:19](=[O:21])=[O:20].O>C1COCC1.CCOCC>[C:12]([C:11]1[C:14]([Cl:18])=[C:15]([CH:16]=[CH:17][C:10]=1[Cl:9])[C:19]([OH:21])=[O:20])#[N:13]

参加物

7

反応物 4

HCID 280Carbon DioxideHCID 962WaterHCID 3031DichlobenilHCID 2724682Lithium diisopropylamide

生成物 1

HCID 540731813-Cyano-2,4-dichlorobenzoic acid

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of lithium di-isopropylamide (2M in heptane, 25 ml) was added to a solution of 2,6-dichlorobenzonitrile (8.6 g) in THF while maintaining the temperature below -70° C. The mixture was stirred for 1.5 hours then poured onto solid carbon dioxide. It was stirred for 1 hour then diluted with ether. Water was added and the mixture was acidified to pH1. It was extracted with ether, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 3-cyano-2,4-dichlorobenzoic acid (9.4 g) as a white solid mp 230°-232° C.

後処理

  1. temperaturewhile maintaining the temperature below -70° C
  2. stirringIt was stirred for 1 hour
  3. extractionIt was extracted with ether
  4. washwashed with water
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness

出典と根拠

ORDレコード
ord-94c6c84eef84410594482a11e584abf1
出典データセット
uspto-grants-1998_05
特許番号
US05747424

関連ノート

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