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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0

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反応

Acetonitrile → 1-(2-Chloro-5-thiazolylmethyl)-3,3-dimethyl-2-nitro-1-phenoxythiocarbonylguanidine

HRID 1657037

印刷プレビュー

反応式

HRID 1657037 の反応式

[Cl:1][C:2]1[S:3][C:4]([CH2:7][NH:8][C:9]([N:14]([CH3:16])[CH3:15])=[N:10][N+:11]([O-:13])=[O:12])=[CH:5][N:6]=1.C([O-])([O-])=O.[K+].[K+].CC#N.[CH:26]1[CH:31]=[CH:30][C:29]([O:32][C:33](Cl)=[S:34])=[CH:28][CH:27]=1>O>[Cl:1][C:2]1[S:3][C:4]([CH2:7][N:8]([C:33]([O:32][C:29]2[CH:30]=[CH:31][CH:26]=[CH:27][CH:28]=2)=[S:34])[C:9]([N:14]([CH3:16])[CH3:15])=[N:10][N+:11]([O-:13])=[O:12])=[CH:5][N:6]=1

参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6342Acetonitrile

HCID 11430Potassium Carbonate

HCID 70498Phenyl thioxochloroformate

HCID 136218199N-(2-chloro-5-thiazolylmethyl)-N',N'-dimethyl-N"-nitroguanidine

生成物 1

HCID 538143491-(2-Chloro-5-thiazolylmethyl)-3,3-dimethyl-2-nitro-1-phenoxythiocarbonylguanidine収率 75.8%

試薬・触媒・溶媒 1

HCID 962

Water

溶媒

実験手順

To a mixture of 1-(2-chloro-5-thiazolylmethyl)-3,3-dimethyl-2-nitroguanidine (200 mg), K2CO3 (420 mg) and CH3CN (13 ml) was added phenyl chlorothionoformate (260 mg) dropwise in 3 minutes at 3° C. under stirring. After stirring at room temperature for 4 hours, water (10 ml) was added to the mixture which was extracted with CHCl3 (20 ml). The organic layer was dried over MgSO4 and evaporated in vacuo. The residue was crystallized from AcOEt-Et2O to afford 230 mg of 1-(2-chloro-5-thiazolylmethyl)-3,3-dimethyl-2-nitro-1-phenoxythiocarbonylguanidine (Compound No. 44) as a white crystal, m.p. 161°-162° C.

後処理

stirringAfter stirring at room temperature for 4 hours
extractionwas extracted with CHCl3 (20 ml)
dry with materialThe organic layer was dried over MgSO4
customevaporated in vacuo
customThe residue was crystallized from AcOEt-Et2O

出典と根拠

ORDレコード: ord-fba465e79bf647b3bec8433209485ee8
出典データセット: uspto-grants-1993_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05256679

反応ノート

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