Potassium Carbonate → HCID 178485057、化合物

HRID 65755

反応式

HRID 65755 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH3:7][N:8]([CH2:10][C:11]1[O:15][C:14]([CH2:16][S:17][CH2:18][CH2:19][NH2:20])=[CH:13][CH:12]=1)[CH3:9].CS[C:23](=[N:27][CH3:28])[NH:24][C:25]#[N:26]>C(#N)C.[N+]([O-])([O-])=O.[Ag+]>[C:25]([N:24]=[C:23]([NH:27][CH3:28])[NH:20][CH2:19][CH2:18][S:17][CH2:16][C:14]1[O:15][C:11]([CH2:10][N:8]([CH3:7])[CH3:9])=[CH:12][CH:13]=1)#[N:26]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 1111031-Cyano-2,3-dimethylisothioureaHCID 1622035-(((2-Aminoethyl)thio)methyl)-N,N-dimethyl-2-furanmethanamine

生成物 1

HCID 178485057HCID 178485057、化合物収率 2.4%

試薬・触媒・溶媒 2

HCID 24470Silver Nitrate触媒HCID 6342Acetonitrile溶媒2 回

実験手順

To a stirred suspension of potassium carbonate (20.7 g) in a solution of 2-[[[5-(dimethylamino)methyl-2-furanyl]methyl]thio]ethanamine (10.7 g) and N-cyano-N'-methylcarbamimidothioic acid methyl ester (7.1 g) in acetonitrile (107 ml) at 70° was added a solution of silver nitrate (9.35 g) in acetonitrile (20 ml) during 1 hr. The mixture was stirred for 16 hr, the solid filtered and the filtrate evaporated to dryness. The residue was dissolved in ethyl acetate (250 ml). A portion of this (10.5 ml) was washed with water (6 ml), the ethyl acetate layer evaporated to give a solid which was crystallised from isopropylacetate (1.75 ml) giving N"-cyano-N-[2-[[[5-(dimethylaminomethyl)-2-furanyl]methyl]thio]ethyl]-N'-methylguanidine (0.35 g) m.p. 79°-81.5°.

後処理

  1. filtrationthe solid filtered
  2. customthe filtrate evaporated to dryness
  3. dissolutionThe residue was dissolved in ethyl acetate (250 ml)
  4. washA portion of this (10.5 ml) was washed with water (6 ml)
  5. customthe ethyl acetate layer evaporated
  6. customto give a solid which
  7. customwas crystallised from isopropylacetate (1.75 ml)

出典と根拠

ORDレコード
ord-318790c9e4144574998bd1b56b0ef298
出典データセット
uspto-grants-1978_12
特許番号
US04128658

関連ノート

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