Ethyl Acetate → methyl 2-[(3-carbamoyl-5-chloro-2-iminopyridin-1(2H)-yl)methyl]-4-chlorobenzoate hydrobromide

HRID 1014018ノート

反応式

HRID 1014018 の反応式
[NH2:1][C:2]1[N:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].[Cl:12][C:13]1[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[C:15]([CH2:23][Br:24])[CH:14]=1.C(OCC)(=O)C>CN(C=O)C>[BrH:24].[C:4]([C:3]1[C:2](=[NH:1])[N:10]([CH2:23][C:15]2[CH:14]=[C:13]([Cl:12])[CH:22]=[CH:21][C:16]=2[C:17]([O:19][CH3:20])=[O:18])[CH:9]=[C:8]([Cl:11])[CH:7]=1)(=[O:5])[NH2:6]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 20814722Methyl 2-(bromomethyl)-4-chlorobenzoateHCID 668768832-Amino-5-chloronicotinamide

生成物 1

HCID 66969549methyl 2-[(3-carbamoyl-5-chloro-2-iminopyridin-1(2H)-yl)methyl]-4-chlorobenzoate hydrobromide収率 15.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

(Step 3) A solution of 2-amino-5-chloronicotinamide (202 mg) and methyl 4-chloro-2-bromomethylbenzoate obtained in Step 2 (470 mg) in DMF (5 ml) was stirred overnight at 90° C. The mixture was allowed to cool to room temperature, ethyl acetate was added, and the precipitated crystals were collected by filtration. The obtained crystals were recrystallized from ethanol and ethyl acetate to give the title compound (78 mg).

後処理

  1. filtrationthe precipitated crystals were collected by filtration
  2. customThe obtained crystals were recrystallized from ethanol and ethyl acetate

出典と根拠

ORDレコード
ord-b16161c4d1ec4d5d994bc74175b31bc4
出典データセット
uspto-grants-2011_07
特許番号
US07982044B2

反応ノート

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