Acetyl chloride → HCID 178487290、化合物

HRID 538081ノート

反応式

HRID 538081 の反応式
[CH3:1][O:2][C:3]1[CH:28]=[CH:27][C:6]2[N:7]([CH3:26])[C:8](=[O:25])[N:9]([CH2:10][C@H:11]3[CH2:16][CH2:15][C@H:14]([C:17]([N:19]4[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]4)=[O:18])[CH2:13][CH2:12]3)[C:5]=2[CH:4]=1.C(N(CC)CC)C.[C:36](Cl)(=[O:38])[CH3:37]>C(Cl)Cl>[C:36]([N:22]1[CH2:21][CH2:20][N:19]([C:17]([C@H:14]2[CH2:15][CH2:16][C@H:11]([CH2:10][N:9]3[C:5]4[CH:4]=[C:3]([O:2][CH3:1])[CH:28]=[CH:27][C:6]=4[N:7]([CH3:26])[C:8]3=[O:25])[CH2:12][CH2:13]2)=[O:18])[CH2:24][CH2:23]1)(=[O:38])[CH3:37]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 178487289HCID 178487289、化合物

生成物 1

HCID 178487290HCID 178487290、化合物収率 64%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5-Methoxy-1-methyl-3-[trans-4-(piperazine-1-carbonyl)-cyclohexylmethyl]-1,3-dihydro-benzoimidazol-2-one (85 mg, 0.22 mmol) was dissolved in anhydrous DCM (4 ml). Triethyl amine (0.12 ml, 0.66 mmol) and acetyl chloride (0.02 ml, 0.26 mmol) were added and the mixture was stirred at room temperature overnight. The solution was washed with saturated NaHCO3 the organic phase was concentrated and the crude product purified on silica column using EtOAc as eluent to give the titled compound (60 mg, 64%).

後処理

  1. washThe solution was washed with saturated NaHCO3 the organic phase
  2. concentrationwas concentrated
  3. customthe crude product purified on silica column

出典と根拠

ORDレコード
ord-f3d6eaa8d3db4c4f800aee9626192a18
出典データセット
uspto-grants-2014_10
特許番号
US08865704B2

反応ノート

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