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HCID 135525218, 화합물 → N-methyl-2-(2-hydroxyphenyl)-2-methoxyiminoacetamide

HRID 432058
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HRID 432058 반응식
[CH3:1][NH:2][C:3](=[O:15])/[C:4](/[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[OH:14])=[N:5]/[O:6][CH3:7].CNC(=O)/C(/C1C=CC=CC=1O)=N\OC>>[CH3:1][NH:2][C:3](=[O:15])[C:4]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[OH:14])=[N:5][O:6][CH3:7]
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참가 물질

3

반응물 2

HCID 135525218HCID 135525218, 화합물HCID 135532297HCID 135532297, 화합물

생성물 1

HCID 136045378N-methyl-2-(2-hydroxyphenyl)-2-methoxyiminoacetamide

실험 절차

9.68 g of crude product (0.0339 mol of methyl E/Z-2-(2-hydroxyphenyl)-2-methoxyimino-acetate, in particular compound II-1c from process step 6, HPLC: 43.7% E isomer of log p=1.48; 29.4% Z isomer of log p=2.37) are dissolved in 100 ml of tetrahydrofuran and cooled to 10° C. With cooling, methylamine is introduced. After about 30 minutes, 50 ml of methanol are added, the solution is saturated with methylamine and the mixture is allowed to stand at 10° C. overnight. The solvents are distilled off under reduced pressure and the residue is mixed with a mixture of 30 ml of 2N hydrochloric acid and 30 ml of saturated sodium chloride solution and extracted three times with 50 ml of ethyl acetate each time. The organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure, giving 8.5 g of crude product which, according to HPLC, contains 52.6% N-methyl-E-2-(2-hydroxyphenyl)-2-methoxyimino-acetamide of log p=0.98 and 31.9% N-methyl-Z-2-(2-hydroxyphenyl)-2-methoxyiminoacetamide of log p=1.29.

출처 및 근거

ORD 기록
ord-20d74a9b4461417b920804ea07d1caa9
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06660872B1

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