Methylamine → HCID 8180193, 화합물

HRID 1782030

반응식

HRID 1782030 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[CH2:11][C:12]([OH:14])=O.C1N=C[N:17](C(N2C=NC=C2)=O)[CH:16]=1.CN.C(OCC)(=O)C>CN(C=O)C.O>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[CH2:11][C:12]([NH:17][CH3:16])=[O:14]

참가 물질

7

반응물 4

HCID 6329MethylamineHCID 8857Ethyl AcetateHCID 682631,1'-CarbonyldiimidazoleHCID 3505552-(2,4-Dimethoxyphenyl)acetic acid

생성물 1

HCID 8180193HCID 8180193, 화합물수율 73.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of (2,4-dimethoxyphenyl)acetic acid (577 mg, 3.0 mmol) and N,N-carbonyldiimidazole (608 mg, 3.75 mmol) in DMF (10 mL) was stirred at room temperature for 45 min, aqueous 40% methyl amine (4.5 mL) was added and the reaction mixture was stirred at room temperature over the week-end. The reaction mixture was is partitoned between ethyl acetate and H2O. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit) to give the subtitled compound (460 mg).

후처리

  1. stirringthe reaction mixture was stirred at room temperature over the week-end
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit)

출처 및 근거

ORD 기록
ord-ef69b6f7495e473da852aa96bc95b40c
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07498338B2

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