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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Dimethylamine → HCID 15907985、化合物

HRID 1268040
ノート
印刷プレビュー

反応式

HRID 1268040 の反応式
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[S:30])[NH:13][C:14]2[CH:27]=[C:26]([Cl:28])[C:17]([O:18][CH2:19][CH2:20]OS(C)(=O)=O)=[C:16]([Cl:29])[CH:15]=2)=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[CH3:31][NH:32][CH3:33]>O1CCCC1.C(OCC)(=O)C>[Cl:28][C:26]1[CH:27]=[C:14]([NH:13][C:12](=[S:30])[NH:11][C:8]2[CH:9]=[CH:10][C:5]([NH:4][C:1](=[O:3])[CH3:2])=[CH:6][CH:7]=2)[CH:15]=[C:16]([Cl:29])[C:17]=1[O:18][CH2:19][CH2:20][N:32]([CH3:33])[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 674DimethylamineHCID 12019007HCID 12019007、化合物

生成物 1

HCID 15907985HCID 15907985、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of methanesulfonic acid 2-{4-[3-(4-acetylamino-phenyl)-thioureido]-2,6-dichlorophenoxy}-ethyl ester (0.33 g) in tetrahydrofuran (6 mL) is added aqueous dimethyl-amine (8.8 M, 0.5 mL) and the mixture is stirred at room temperature for 5 days. The reaction mixture is then diluted with ethyl acetate, then washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. After removal of the solvent under reduced pressure the residue is chromatographed over silica gel (pure methanol is used as the eluant). Pooled product containing fractions are evaporated under reduced pressure and the residue is recrystallized from acetonitrile to provide the desired product as a white powder.

後処理

  1. washwashed with saturated aqueous sodium chloride
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customAfter removal of the solvent under reduced pressure the residue
  4. customis chromatographed over silica gel (pure methanol
  5. additionPooled product containing fractions
  6. customare evaporated under reduced pressure
  7. customthe residue is recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-3ac58aff7f7f4bf1a18f6d4daae7cb2d
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06555561B2

反応ノート

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