Potassium Carbonate → n-(3-((2-Chlorothiazol-5-yl)methyl)-5-methyl-1,3,5-oxadiazinan-4-ylidene)nitramide

HRID 1386818ノート

反応式

HRID 1386818 の反応式
[Cl:1][C:2]1[S:3][C:4]([CH2:7]I)=[CH:5][N:6]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:15][N:16]1[C:21](=[N:22][N+:23]([O-:25])=[O:24])[NH:20][CH2:19][O:18][CH2:17]1>CN(C)C=O>[Cl:1][C:2]1[S:3][C:4]([CH2:7][N:20]2[CH2:19][O:18][CH2:17][N:16]([CH3:15])[C:21]2=[N:22][N+:23]([O-:25])=[O:24])=[CH:5][N:6]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 98166342-Chloro-5-(iodomethyl)thiazoleHCID 136277959N-(3-methyl-1,3,5-oxadiazinan-4-ylidene)nitramide

生成物 1

HCID 107646n-(3-((2-Chlorothiazol-5-yl)methyl)-5-methyl-1,3,5-oxadiazinan-4-ylidene)nitramide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

A mixture of 2.0 g of 2-chloro-5-iodomethyl-thiazole, 20 ml of dimethylformamide, 2.66 g of potassium carbonate and 1.23 g of 3-methyl-4-nitroimino-perhydro-1,3,5-oxadiazine is stirred for 16 hours at 50° C., cooled to room temperature and filtered; the filtrate is concentrated to dryness by evaporation. The residue is purified by column chromatography on silica gel using dichloromethane/methanol (9:1), yielding the title compound having a melting point of 132-134° C.

後処理

  1. temperaturecooled to room temperature
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated to dryness by evaporation
  4. customThe residue is purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-528c66170e6b4e0f88773a99109ec934
出典データセット
uspto-grants-2001_07
特許番号
US06265585B1

反応ノート

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