Benzoyl chloride → HCID 14277502、化合物

HRID 1461749ノート

反応式

HRID 1461749 の反応式
[C:1](Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:10][C@H:11]1[CH2:25][C@H:24]2[C@@H:14]([CH2:15][C:16]3[C:26]4[C:19](=[CH:20][CH:21]=[CH:22][C:23]2=4)[NH:18][CH:17]=3)[N:13]([CH2:27][CH2:28][CH3:29])[CH2:12]1>C(Cl)Cl.C(N(CC)CC)C>[C:1]([NH:10][C@H:11]1[CH2:25][C@H:24]2[C@@H:14]([CH2:15][C:16]3[C:26]4[C:19](=[CH:20][CH:21]=[CH:22][C:23]2=4)[NH:18][CH:17]=3)[N:13]([CH2:27][CH2:28][CH3:29])[CH2:12]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 7412Benzoyl chlorideHCID 134688038alpha-Amino-6-n-propylergoline

生成物 1

HCID 14277502HCID 14277502、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine溶媒

反応条件

温度
20 °C

実験手順

1.4 ml benzoylchloride in 5 ml CH2Cl2 are added drop-wise with stirring at 5°-10° C. to a suspension of 3.0 g 8α-amino-6-n-propylergoline in 100 ml CH2Cl2 and 2.0 ml triethylamine. The obtained reaction mixture is stirred for 15 to 20 hours at 20° C. and then washed thoroughly 2× with 25 ml 2N NaOH and H2O. The organic phase is dried over MgSO4, filtered and evaporated. The residue (pale brown foam) is dissolved in ethanol, and crystallised as the hydrobromide by addition of equivalent amounts of HBr in acetic acid. M.P. on recrystallisation from C2H5OH/H2O (80:2)=290° with decomposition.

後処理

  1. customThe obtained reaction mixture
  2. washwashed thoroughly 2× with 25 ml 2N NaOH and H2O
  3. dry with materialThe organic phase is dried over MgSO4
  4. filtrationfiltered
  5. customevaporated
  6. dissolutionThe residue (pale brown foam) is dissolved in ethanol
  7. customcrystallised as the hydrobromide by addition of equivalent amounts of HBr in acetic acid
  8. customM.P. on recrystallisation from C2H5OH/H2O (80:2)=290° with decomposition

出典と根拠

ORDレコード
ord-9012bb01317a4757b0e5e9c0ea6ce225
出典データセット
uspto-grants-1991_12
特許番号
US05077298

反応ノート

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