N-Methylhomoveratrylamine → 3,4-Dichloro-N-[4-[[2-(3,4-dimethoxyphenyl)ethyl]methylamino]butyl]-N-(1-methylethyl)benzenesulfonamide

HRID 2290955

反応式

HRID 2290955 の反応式
[CH:1]([N:4]([CH2:16][CH2:17][CH2:18][CH:19]=O)[S:5]([C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[C:10]([Cl:15])[CH:9]=1)(=[O:7])=[O:6])([CH3:3])[CH3:2].[CH3:21][NH:22][CH2:23][CH2:24][C:25]1[CH:34]=[CH:33][C:30]([O:31][CH3:32])=[C:27]([O:28][CH3:29])[CH:26]=1>C(O)C.O=[Pt]=O>[Cl:15][C:10]1[CH:9]=[C:8]([S:5]([N:4]([CH2:16][CH2:17][CH2:18][CH2:19][N:22]([CH2:23][CH2:24][C:25]2[CH:34]=[CH:33][C:30]([O:31][CH3:32])=[C:27]([O:28][CH3:29])[CH:26]=2)[CH3:21])[CH:1]([CH3:2])[CH3:3])(=[O:6])=[O:7])[CH:13]=[CH:12][C:11]=1[Cl:14]

参加物

5

反応物 2

HCID 77039N-MethylhomoveratrylamineHCID 13770967N-isopropyl-N-(4-oxobutyl)-3,4-dichlorobenzenesulfonamide

生成物 1

HCID 137709683,4-Dichloro-N-[4-[[2-(3,4-dimethoxyphenyl)ethyl]methylamino]butyl]-N-(1-methylethyl)benzenesulfonamide

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 702Ethanol溶媒

実験手順

The aldehyde prepared in the preceding paragraph (8.90 g, 0.027 m) and N-methyl-homoveratrylamine (5.29 g, 0.027 m) in absolute ethanol (100 ml) containing PtO2 (0.6 g) was shaken under hydrogen (7 hours) and the reaction filtered and stripped to provide the crude product (13.32 g) as a dark greenish gum. This material was chromatographed, after removal of a small amount of insoluble solid, on dry column silica gel (500 g) with 30% methanol/70% ethyl acetate to provide the title compound (7.26 g) as a clear white gum.

後処理

  1. filtrationthe reaction filtered
  2. customto provide the crude product (13.32 g) as a dark greenish gum
  3. customThis material was chromatographed
  4. customafter removal of a small amount of insoluble solid
  5. dry with materialon dry column silica gel (500 g) with 30% methanol/70% ethyl acetate

出典と根拠

ORDレコード
ord-fe203a9032f446659f56f459b8ba90a1
出典データセット
uspto-grants-1986_10
特許番号
US04618711

関連ノート

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