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

HRID 51842

反応式

HRID 51842 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1ea0648519114dda86f440fe12a9734a
出典データセット
uspto-grants-2004_03
特許番号
US06713499B2

関連ノート

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