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

HRID 2414260노트

반응식

HRID 2414260 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d4526409a12a456bb193fe73c51b7090
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06812229B1

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