Ethanol → HCID 67154551、化合物

HRID 83064ノート

反応式

HRID 83064 の反応式
[Cl:1]C(OC(Cl)C)=O.C([N:21]1[CH2:24][CH:23]([C:25]2[O:26][C:27]3[CH:33]=[CH:32][CH:31]=[CH:30][C:28]=3[CH:29]=2)[CH2:22]1)(C1C=CC=CC=1)C1C=CC=CC=1.C(O)C>ClCCl>[ClH:1].[O:26]1[C:27]2[CH:33]=[CH:32][CH:31]=[CH:30][C:28]=2[CH:29]=[C:25]1[CH:23]1[CH2:22][NH:21][CH2:24]1

参加物

5

反応物 3

HCID 702EthanolHCID 5213051-Chloroethyl chloroformateHCID 671547231-Benzhydryl-3-(benzofuran-2-yl)azetidine

生成物 1

HCID 67154551HCID 67154551、化合物収率 123%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

1-Chloroethyl chloroformate (36 μL, 0.33 mmol) was added to a solution of 1-benzhydryl-3-(benzofuran-2-yl)azetidine (108 mg, 0.32 mmol) in dichloromethane (3 mL) at 0° C. The reaction mixture was stirred for 2 hours at 0° C. and for 1 hour at room temperature. Ethanol (3 mL) was added at 0° C. and the reaction mixture was stirred for 2 hours at 0° C., for 19 hours at room temperature and for 4 hours at 40° C. After concentration to dryness, the crude mixture was triturated in n-pentane (2×4 mL) to afford the title compound as a pink solid (82 mg, 123%) which was used without further purification.

後処理

  1. stirringthe reaction mixture was stirred for 2 hours at 0° C., for 19 hours at room temperature and for 4 hours at 40° C
  2. concentrationAfter concentration to dryness
  3. customthe crude mixture was triturated in n-pentane (2×4 mL)

出典と根拠

ORDレコード
ord-7acbd87f55b0475fb9dc0b07e31c566c
出典データセット
uspto-grants-2014_09
特許番号
US08846711B2

反応ノート

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