Sodium Methoxide → {2-Methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea

HRID 51842

반응식

HRID 51842 반응식
C([NH:9][C:10]([NH:12][C:13]1[CH:18]=[C:17]([N:19]([CH2:21][CH2:22][O:23][CH3:24])[CH3:20])[CH:16]=[CH:15][C:14]=1[O:25][CH3:26])=[S:11])(=O)C1C=CC=CC=1.C[O-].[Na+]>CO>[CH3:26][O:25][C:14]1[CH:15]=[CH:16][C:17]([N:19]([CH2:21][CH2:22][O:23][CH3:24])[CH3:20])=[CH:18][C:13]=1[NH:12][C:10]([NH2:9])=[S:11]

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 220157361-Benzoyl-3-{2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea

생성물 1

HCID 22015743{2-Methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea수율 97%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a stirred suspension of 2.00 g (5.36 mmol) 1-benzoyl-3-{2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea in 13 ml methanol was added dropwise 0.15 ml (0.80 mmol) 5.4 M sodium methylate solution and stirring continued for 1 h at room temperature. The mixture was then poured onto water and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated in vacuo. Flash chromatography (ethyl acetate) afforded 1.40 g (97%) {2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea as an amber oil. ES-MS m/e (%): 270 (M+H+, 100).

후처리

  1. additionThe mixture was then poured onto water
  2. extractionextracted three times with ethyl acetate
  3. dry with materialThe combined organic phases were dried over sodium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-1ea0648519114dda86f440fe12a9734a
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713499B2

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