Methanol → Methyl 4-chloro-3-(methoxycarbonylaminomethyl)benzoate

HRID 2414260ノート

反応式

HRID 2414260 の反応式
Br[CH2:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[Cl:13])[C:6]([O:8][CH3:9])=[O:7].[O-:14][C:15]#[N:16].[K+].CO.CN(C)[CH:22]=[O:23]>C(OCC)(=O)C.O>[Cl:13][C:12]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[CH2:2][NH:16][C:15]([O:23][CH3:22])=[O:14]

参加物

7

反応物 4

HCID 887MethanolHCID 6228DimethylformamideHCID 11378442Potassium cyanateHCID 12144656Methyl 3-(bromomethyl)-4-chlorobenzoate

生成物 1

HCID 22645128Methyl 4-chloro-3-(methoxycarbonylaminomethyl)benzoate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

16.0 g of the obtained methyl 3-bromomethyl-4-chlorobenzoate, 15.0 g of potassium cyanate and 35 ml of methanol were added to 200 ml of N,N-dimethylformamide, followed by stirring at 90° C. for 4 hours. After completion of the reaction, water was added to the reaction mixture, extraction with ethyl acetate was carried out, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the obtained crude crystals were washed with isopropanol to obtain 25.2 g of methyl 4-chloro-3-(methoxycarbonylaminomethyl)benzoate as white crystals.

後処理

  1. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  2. distillationThe solvent was distilled off under reduced pressure
  3. customthe obtained crude crystals
  4. washwere washed with isopropanol

出典と根拠

ORDレコード
ord-d4526409a12a456bb193fe73c51b7090
出典データセット
uspto-grants-2004_11
特許番号
US06812229B1

反応ノート

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