Ammonium Chloride → HCID 18679742、化合物

HRID 1633716

反応式

HRID 1633716 の反応式
I[C:2]1[N:3]=[CH:4][N:5]([S:7]([N:10]([CH3:12])[CH3:11])(=[O:9])=[O:8])[CH:6]=1.C([Mg]Br)C.[CH3:17][O:18][C:19]1[C:20]([N+:30]([O-:32])=[O:31])=[C:21]2[C:26](=[CH:27][CH:28]=1)[C:25](=[O:29])[CH2:24][CH2:23][CH2:22]2.[Cl-].[NH4+]>ClCCl>[OH:29][C:25]1([C:2]2[N:3]=[CH:4][N:5]([S:7]([N:10]([CH3:12])[CH3:11])(=[O:9])=[O:8])[CH:6]=2)[C:26]2[C:21](=[C:20]([N+:30]([O-:32])=[O:31])[C:19]([O:18][CH3:17])=[CH:28][CH:27]=2)[CH2:22][CH2:23][CH2:24]1

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 2773390N,N-Dimethyl 4-iodo-1H-imidazole-1-sulfonamideHCID 130673376-Methoxy-5-nitro-1,2,3,4-tetrahydronaphthalen-1-oneHCID 178418443HCID 178418443、化合物

生成物 1

HCID 18679742HCID 18679742、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 4-iodo-N,N-dimethyl-1H-imidazole-1-sulfonamide (3.0 g, 10 mmol) (R. M. Turner, J. Org. Chem. (1991), 56, 5739-5740) in dichloromethane (40 mL) was treated with ethyl magnesium bromide (3.0M in diethyl ether, 3.3 mL) over 5 minutes, stirred for 30 minutes, treated with 6-methoxy-5-nitro-1-tetralone (2.6 g, 11.8 mmol), stirred for 16 hours, treated with ammonium chloride solution and extracted with dichloromethane. The extract was dried (MgSO4), filtered and concentrated to provide the desired compound.

後処理

  1. stirringstirred for 16 hours
  2. extractionextracted with dichloromethane
  3. dry with materialThe extract was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-ef094213dff74786b4547236844aa51b
出典データセット
uspto-grants-2003_01
特許番号
US06503935B1

関連ノート

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