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

HRID 1734112노트

반응식

HRID 1734112 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c8087508363c49c39cbd8964f431febf
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532267

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