O-[(5-chlorothiophen-2-yl)methyl]hydroxylamine → HCID 53817257、化合物

HRID 621373ノート

反応式

HRID 621373 の反応式
[Cl:1][C:2]1[S:6][C:5]([CH2:7][O:8][NH2:9])=[CH:4][CH:3]=1.[C:10]([C:13]1[C:14](=[O:29])[CH2:15][CH:16]([CH:23]2[CH2:28][CH2:27][CH2:26][S:25][CH2:24]2)[CH2:17][C:18]=1[O:19][C:20](=[O:22])[CH3:21])(=O)[CH3:11]>C(O)C>[C:20]([O:19][C:18]1[CH2:17][CH:16]([CH:23]2[CH2:28][CH2:27][CH2:26][S:25][CH2:24]2)[CH2:15][C:14](=[O:29])[C:13]=1[C:10](=[N:9][O:8][CH2:7][C:5]1[S:6][C:2]([Cl:1])=[CH:3][CH:4]=1)[CH3:11])(=[O:22])[CH3:21]

参加物

4

反応物 2

HCID 10986580O-[(5-chlorothiophen-2-yl)methyl]hydroxylamineHCID 20043437HCID 20043437、化合物

生成物 1

HCID 53817257HCID 53817257、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.34 g (2.0 mmol) of (5-chlorothien-2-yl)methoxyamine is added to a stirred solution of 0.59 g (2.0 mmol) of 2-acetyl-3-acetyloxy-5-(tetrahydro-2H-thiopyran-3-yl)-cyclohex-2-en-1-one in 10 ml of absolute ethanol. After stirring overnight at room temperature, the reaction mixture is concentrated under reduced pressure. The resulting residue is diluted with 25 ml of dichloromethane and washed twice with 10 ml of saturated sodium chloride solution. The washed extract is then dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The product can then be purified by column chromatography employing tetrahydrofuran-hexane (1:2 by volume) as eluent to afford the title compound.

後処理

  1. concentrationthe reaction mixture is concentrated under reduced pressure
  2. additionThe resulting residue is diluted with 25 ml of dichloromethane
  3. washwashed twice with 10 ml of saturated sodium chloride solution
  4. extractionThe washed extract
  5. dry with materialis then dried over anhydrous magnesium sulfate
  6. customevaporated under reduced pressure
  7. customThe product can then be purified by column chromatography

出典と根拠

ORDレコード
ord-6cfb4e42b38645c9a88eece31c22e175
出典データセット
uspto-grants-1989_04
特許番号
US04824470

反応ノート

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