Triethylamine → 1,2-Dihydro-8-(dimethylamino)methylbenzo[b]pyrrolo[3,2,1-jk][1,2,4]triazolo[4,3-d][1,4]benzodiazepine

HRID 2050999ノート

反応式

HRID 2050999 の反応式
[CH2:1]1[N:12]2[C:13]3[C:3](=[CH:4][CH:5]=[CH:6][C:7]=3[C:8](=S)[NH:9][C:10]3[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=32)[CH2:2]1.Cl.CN(C[C:24]([NH:26][NH2:27])=O)C.[CH2:28]([N:30]([CH2:33]C)[CH2:31]C)C>CN(C)C=O>[CH3:28][N:30]([CH2:33][C:15]1[CH:16]=[CH:17][C:10]2[N:9]3[CH:24]=[N:26][N:27]=[C:8]3[C:7]3[CH2:6][CH2:5][CH:4]=[C:3]4[CH:2]=[CH:1][N:12]([C:13]=34)[C:11]=2[CH:14]=1)[CH3:31]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 68318N,N-Dimethylglycine hydrazide hydrochlorideHCID 15132539HCID 15132539、化合物

生成物 1

HCID 679230661,2-Dihydro-8-(dimethylamino)methylbenzo[b]pyrrolo[3,2,1-jk][1,2,4]triazolo[4,3-d][1,4]benzodiazepine収率 47.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1,2-Dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin6-thione (4 g) was added to a solution of dimethylaminoacetic hydrazide hydrochloride (2 g) and triethylamine (2.4 ml) in dimethylformamide (25 ml). The mixture was refluxed overnight, cooled, and concentrated under reduced pressure. The residue was purified by high performance liquid chromatography (2.5% methano/dichloromethane). The appropriate fractions were triturated with dry ether to yield 2.4 g (47.2%) of product, mp 164°-165° C.

後処理

  1. temperatureThe mixture was refluxed overnight
  2. temperaturecooled
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by high performance liquid chromatography (2.5% methano/dichloromethane)
  5. customThe appropriate fractions were triturated with dry ether

出典と根拠

ORDレコード
ord-261a1c550af5459ba45f8471822a41d2
出典データセット
uspto-grants-1991_05
特許番号
US05015738

反応ノート

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