Triethylamine → HCID 18546092、化合物

HRID 1267214ノート

反応式

HRID 1267214 の反応式
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([C:8](Cl)=[O:9])[S:4][N:3]=1.[NH2:11][CH:12]([CH:15]([CH3:17])[CH3:16])[C:13]#[N:14].C(N(CC)CC)C>ClCCl>[C:13]([CH:12]([NH:11][C:8]([C:5]1[S:4][N:3]=[C:2]([Cl:1])[C:6]=1[Cl:7])=[O:9])[CH:15]([CH3:17])[CH3:16])#[N:14]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 104191372-Amino-3-methylbutyronitrileHCID 109768863,4-Dichloro-5-isothiazolecarbonyl chloride

生成物 1

HCID 18546092HCID 18546092、化合物収率 55.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 3,4-dichloro-5-isothiazolecarboxylic acid chloride (2.1 g) in dichloro-methane (5 ml) was added drop by drop to a solution of 2-amino-3-methyl-butyronitrile (1.2 g) and triethylamine (1.5 g) in dichloromethane (10 ml) under ice cooling. After the addition was completed, the temperature was brought to room temperature, and the mixture was stirred for further 4 hours. The reaction mixture was then washed with water and dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the remaining residue was purified by silica gel column chromatography (eluent: chloroformn) to obtain N-(1-cyano-2-methyl-propyl)-3,4-dichloro-5-isothiazolecarboxamide (1.5 g) (mp 120-121° C.).

後処理

  1. additionAfter the addition
  2. customwas brought to room temperature
  3. washThe reaction mixture was then washed with water
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe remaining residue was purified by silica gel column chromatography (eluent: chloroformn)

出典と根拠

ORDレコード
ord-dfb2a1fd6a8d4420a8e434bf90b4f0de
出典データセット
uspto-grants-2003_04
特許番号
US06552056B2

反応ノート

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