Water → HCID 54343145、化合物

HRID 1780007ノート

反応式

HRID 1780007 の反応式
Cl[CH2:2][C:3](=[O:18])[C:4]([NH:7][C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[CH:10]=1)([CH3:6])[CH3:5].[C-:19]#[N:20].[Na+].O.C(Cl)Cl>C(#N)C.C1OCCOCCOCCOCCOCCOC1>[C:19]([CH2:2][C:3](=[O:18])[C:4]([NH:7][C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[CH:10]=1)([CH3:6])[CH3:5])#[N:20]

参加物

7

反応物 4

HCID 962WaterHCID 6344DichloromethaneHCID 8929Sodium CyanideHCID 54029353HCID 54029353、化合物

生成物 1

HCID 54343145HCID 54343145、化合物収率 43%

試薬・触媒・溶媒 2

HCID 2855718-Crown-6触媒HCID 6342Acetonitrile溶媒

実験手順

N-(3'-chloro-1',1'-dimethylacetonyl)-3,5-dichlorobenzamide (30 gm, 0.0972 m), sodium cyanide (15 gm, 0,306 m) and 18-crown-6 (1 gm) were dissolved in 300 ml of acetonitrile in a round bottom flask under a nitrogen atmosphere. The mixture was heated to reflux for about 4 hours. The contents of the flask were then cooled and transferred to a separatory funnel along with 100 ml of water and 500 ml of methylene chloride and mixed well. The aqueous layer was discarded and the organic layer was washed sequentially with water and brine, dried and the solvents stripped off to yield 12.5 gm of the product after recrystallization from methylene chloride and hexane.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for about 4 hours
  3. temperatureThe contents of the flask were then cooled
  4. additionmixed well
  5. washthe organic layer was washed sequentially with water and brine
  6. customdried

出典と根拠

ORDレコード
ord-82704ab6fb5e402c880403cdca9aad72
出典データセット
uspto-grants-1997_05
特許番号
US05629346

反応ノート

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