Triethylamine → HCID 18546092, 화합물

HRID 1267214노트

반응식

HRID 1267214 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 18546092HCID 18546092, 화합물수율 55.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.).

후처리

  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)

출처 및 근거

ORD 기록
ord-dfb2a1fd6a8d4420a8e434bf90b4f0de
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06552056B2

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