Water → HCID 66877344、化合物

HRID 447873

反応式

HRID 447873 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:3]=1[C:4]#[N:5].CN(C1C=CC=CN=1)C.[C:20](Cl)(=[O:28])[O:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.O>CC(N(C)C)=O>[Cl:10][C:7]1[CH:8]=[CH:9][C:2]([NH:1][C:20](=[O:28])[O:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[C:3]([C:4]#[N:5])[CH:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 15891Phenyl chloroformateHCID 218852-DimethylaminopyridineHCID 800192-Amino-5-chlorobenzonitrile

生成物 1

HCID 66877344HCID 66877344、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

(Step 1) To a solution of 2-amino-5-chlorobenzonitrile (5.0 g) and dimethylaminopyridine (0.12 g) in dimethylacetamide (25 ml) was added dropwise phenyl chlorocarbonate (6.2 ml) at room temperature, and the mixture was stirred overnight. The reaction mixture was poured into water, and extracted twice with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtered. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5-*3:7) to give phenyl (4-chloro-2-cyanophenyl)carbamate (7.04 g).

後処理

  1. extractionextracted twice with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5-*3:7)

出典と根拠

ORDレコード
ord-12c4fe8d2eb34c0e938d9981a8796f9c
出典データセット
uspto-grants-2013_07
特許番号
US08481569B2

関連ノート

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