Dimethylformamide → 6-Amidino-2-naphthyl 5-(4-carboxybutyrylaminomethyl)furan-2-carboxylate methanesulfonate

HRID 1734112ノート

反応式

HRID 1734112 の反応式
CN(C=O)C.Cl.[C:7]([CH2:10][CH2:11][CH2:12][C:13]([NH:15][CH2:16][C:17]1[O:21][C:20]([C:22]([O:24][C:25]2[CH:34]=[CH:33][C:32]3[C:27](=[CH:28][CH:29]=[C:30]([C:35](=[NH:37])[NH2:36])[CH:31]=3)[CH:26]=2)=[O:23])=[CH:19][CH:18]=1)=[O:14])([OH:9])=[O:8].[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]>CC(C)=O>[CH3:38][S:39]([OH:42])(=[O:41])=[O:40].[C:7]([CH2:10][CH2:11][CH2:12][C:13]([NH:15][CH2:16][C:17]1[O:21][C:20]([C:22]([O:24][C:25]2[CH:34]=[CH:33][C:32]3[C:27](=[CH:28][CH:29]=[C:30]([C:35](=[NH:36])[NH2:37])[CH:31]=3)[CH:26]=2)=[O:23])=[CH:19][CH:18]=1)=[O:14])([OH:9])=[O:8]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 6395Methanesulfonic AcidHCID 98254776-Amidino-2-naphthyl 5-(4-carboxybutyrylaminomethyl)furan-2-carboxylate hydrochloride

生成物 1

HCID 223988436-Amidino-2-naphthyl 5-(4-carboxybutyrylaminomethyl)furan-2-carboxylate methanesulfonate収率 68.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To 10 ml of DMF was added 2.0 g of 6-amidino-2-naphthyl 5-(4-carboxybutyrylaminomethyl)furan-2-carboxylate hydrochloride, then 4.6 g of methanesulfonic acid was added dropwise while cooling with ice, and the mixture was stirred for 10 minutes. Then, the mixture was added in small portions into 400 ml of acetone and stirred for 4 hours while cooling with ice. The supernatant was decanted, 1 l of ether was added to the residue and stirred, and the precipitate was collected by filtration to obtain 1.54 g of the intended product.

後処理

  1. temperaturewhile cooling with ice
  2. stirringstirred for 4 hours
  3. temperaturewhile cooling with ice
  4. customThe supernatant was decanted
  5. addition1 l of ether was added to the residue
  6. stirringstirred
  7. filtrationthe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-c8087508363c49c39cbd8964f431febf
出典データセット
uspto-grants-1996_07
特許番号
US05532267

反応ノート

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