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Hydrochloric Acid → 1-(4-chloro-2-fluoro-5-bis(methanesulphonyl) amino-phenyl)-4,5-dicyano-3-difluoromethyl-1,3-dihydro-2H-imidazol-2-one

HRID 465699
ノート
印刷プレビュー

反応式

HRID 465699 の反応式
ClC1C(OCC#C)=CC(N2C(C#N)=C(C#N)N(CCC)C2=O)=C(F)C=1.[Cl:26][C:27]1[C:32]([N+:33]([O-])=O)=[CH:31][C:30]([N:36]2[C:40]([C:41]#[N:42])=[C:39]([C:43]#[N:44])[N:38]([CH:45]([F:47])[F:46])[C:37]2=[O:48])=[C:29]([F:49])[CH:28]=1.C(N(CC)CC)C.[CH3:57][S:58](Cl)(=[O:60])=[O:59].Cl>ClCCl>[Cl:26][C:27]1[C:32]([N:33]([S:58]([CH3:57])(=[O:60])=[O:59])[S:58]([CH3:57])(=[O:60])=[O:59])=[CH:31][C:30]([N:36]2[C:40]([C:41]#[N:42])=[C:39]([C:43]#[N:44])[N:38]([CH:45]([F:47])[F:46])[C:37]2=[O:48])=[C:29]([F:49])[CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 198752181-(4-chloro-2-fluoro-5-nitrophenyl)-4,5-dicyano-3-difluoromethyl-1,3-dihydro-2H-imidazol-2-oneHCID 198752701-(4-chloro-2-fluoro-5-propargyloxyphenyl)-4,5-dicyano-3-propyl-1,3-dihydro-2H-imidazol-2-one

生成物 1

HCID 19875281
1-(4-chloro-2-fluoro-5-bis(methanesulphonyl) amino-phenyl)-4,5-dicyano-3-difluoromethyl-1,3-dihydro-2H-imidazol-2-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The product of Example 77, 1-(4-chloro-2-fluoro-5-nitrophenyl)-4,5-dicyano-3-difluoromethyl-1,3-dihydro-2H-imidazol-2-one, (0.7 g, 2.1 mmol) is dissolved in dichloromethane and treated sequentially at 0° C. with triethylamine (0.27 g, 2.8 mmol) and methanesulphonyl chloride (0.28 g, 2.5 mmol). The solution is allowed to stir 16 hours at ambient temperature, then poured onto 10 mL of 1N hydrochloric acid solution. The organic layer is separated, washed with brine, and dried and concentrated via standard techniques to furnish 1-(4-chloro-2-fluoro-5-methanesulphonylaminophenyl) -4,5-dicyano-3-difluoromethyl-1,3-dihydro-2H-imidazol-2-one (VI).

後処理

  1. customThe organic layer is separated
  2. washwashed with brine
  3. customdried
  4. concentrationconcentrated via standard techniques

出典と根拠

ORDレコード
ord-66326e650ab448b5a6ae28a4a8351396
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05153316

反応ノート

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