1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 19810407、化合物

HRID 373497

反応式

HRID 373497 の反応式
Cl.CN(C)CCCN=C=NCC.[C:13]([O:17][C:18]([C:20]1[CH:28]=[CH:27][C:23]([C:24]([OH:26])=O)=[CH:22][CH:21]=1)=[O:19])([CH3:16])([CH3:15])[CH3:14].[CH3:29][CH:30]([S:32]([NH2:35])(=[O:34])=[O:33])[CH3:31]>CN(C)C1C=CN=CC=1.ClCCl.C(OCC)(=O)C>[CH:30]([S:32]([NH:35][C:24]([C:23]1[CH:22]=[CH:21][C:20]([C:18]([O:17][C:13]([CH3:14])([CH3:15])[CH3:16])=[O:19])=[CH:28][CH:27]=1)=[O:26])(=[O:34])=[O:33])([CH3:31])[CH3:29]

参加物

7

反応物 3

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27609544-(tert-Butoxycarbonyl)benzoic acidHCID 3549191Propane-2-sulfonamide

生成物 1

HCID 19810407HCID 19810407、化合物収率 74.1%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (198 mg) was added to a stirred mixture of 4-(t-butoxycarbonyl)benzoic acid (195 mg), 2-propanesulfonamide (98 mg) and 4-dimethylaminopyridine (126 mg) in dichloromethane (3.7 ml). The mixture was stirred overnight, diluted with ethyl acetate, washed (1N HCl, brine), dried (MgSO4), and evaporated. The crude product was purified by flash chromatography, eluting with acetone:hexanes (75:25), to afford the product (193 mg): TLC, Rf =0.64, acetone:hexanes (75:25): MS, m/e=356(M+29), 330(M+3), 329(M+2), 328(M+1), 272, 223, 222, 205, 204, 166.

後処理

  1. washwashed (1N HCl, brine)
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customThe crude product was purified by flash chromatography
  5. washeluting with acetone:hexanes (75:25)

出典と根拠

ORDレコード
ord-399b20e674fb4381b5e6e750f26db590
出典データセット
uspto-grants-1992_11
特許番号
US05164371

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