Triethylamine → HCID 178477733、化合物

HRID 2379859ノート

反応式

HRID 2379859 の反応式
Cl.Cl.[NH2:3][CH2:4][C:5]1[S:6][CH:7]=[C:8]([C:10]2[N:11]=[C:12]([N:15]=[C:16]([NH2:18])[NH2:17])[S:13][CH:14]=2)[N:9]=1.[CH2:19]([S:21](C(=N)OCC)(=[O:23])=[O:22])[CH3:20].[CH2:29]([N:31](CC)CC)C>CO>[NH2:17][C:16](=[N:15][C:12]1[S:13][CH:14]=[C:10]([C:8]2[N:9]=[C:5]([CH2:4][NH:3][CH:29]=[N:31][S:21]([CH2:19][CH3:20])(=[O:22])=[O:23])[S:6][CH:7]=2)[N:11]=1)[NH2:18]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 189538344-(2-Aminomethylthiazol-4-yl)-2-(diaminomethyleneamino)thiazole dihydrochlorideHCID 18953866Ethyl ethanesulfonylformimidate

生成物 1

HCID 178477733HCID 178477733、化合物収率 35.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A suspension of 4-(2-aminomethylthiazol-4-yl)-2-(diaminomethyleneamino)thiazole dihydrochloride (1.3 g), ethyl ethanesulfonylformimidate (0.8 g) and triethylamine (1.0 g) in methanol (20 ml) was stirred at room temperature for 8 hours. The solvent was removed under reduced pressure. The residue was chromatographed on a silica gel column eluting with a mixture of chloroform and methanol (10:1). Recrystallization from a mixture of N,N-dimethylformamide and water afforded 2-(diaminomethyleneamino)-4-(2-ethanesulfonyliminomethylaminomethylthiazol-4-yl)thiazole (0.53 g).

後処理

  1. customThe solvent was removed under reduced pressure
  2. customThe residue was chromatographed on a silica gel column
  3. washeluting with a mixture of chloroform and methanol (10:1)
  4. customRecrystallization
  5. additionfrom a mixture of N,N-dimethylformamide and water

出典と根拠

ORDレコード
ord-961f49455de241f3b6258f1f0f1f0b5a
出典データセット
uspto-grants-1994_11
特許番号
US05364871

反応ノート

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