O-[(5-chlorothiophen-2-yl)methyl]hydroxylamine → HCID 136127206、化合物

HRID 621370ノート

反応式

HRID 621370 の反応式
[C:1]([C:4]1[C:5](=[O:17])[CH2:6][CH:7]([CH:11]2[CH2:16][CH2:15][CH2:14][S:13][CH2:12]2)[CH2:8][C:9]=1[OH:10])(=O)[CH3:2].[Cl:18][C:19]1[S:23][C:22]([CH2:24][O:25][NH2:26])=[CH:21][CH:20]=1>C(O)C>[Cl:18][C:19]1[S:23][C:22]([CH2:24][O:25][N:26]=[C:1]([C:4]2[C:5](=[O:17])[CH2:6][CH:7]([CH:11]3[CH2:16][CH2:15][CH2:14][S:13][CH2:12]3)[CH2:8][C:9]=2[OH:10])[CH3:2])=[CH:21][CH:20]=1

参加物

4

反応物 2

HCID 10986580O-[(5-chlorothiophen-2-yl)methyl]hydroxylamineHCID 15614621HCID 15614621、化合物

生成物 1

HCID 136127206HCID 136127206、化合物収率 95%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution containing 5.1 g (0.020 mol) of 2-acetyl-3-hydroxy-5-(tetrahydro-2H-thiopyran-3-yl)cyclohex-2-en-1-one and 3.4 g (0.021 mol) of (5-chlorothien-2-yl)methoxyamine in 200 ml of ethanol was stirred overnight (about 14 hours) at room temperature and then evaporated to remove ethanol. The concentrate was diluted with 150 ml of methylene chloride and then washed with 100 ml of water and then with 100 ml of saturated aqueous sodium chloride solution. The washed methylene chloride solution was dried over anhydrous magnesium sulfate and then evaporated to dryness under reduced pressure to afford a white solid. Recrystallation of this solid with absolute ethanol afforded 7.6 g of the title compound, m.p. 154°-155° C. cl EXAMPLE 2

後処理

  1. customevaporated
  2. customto remove ethanol
  3. additionThe concentrate was diluted with 150 ml of methylene chloride
  4. washwashed with 100 ml of water
  5. dry with materialThe washed methylene chloride solution was dried over anhydrous magnesium sulfate
  6. customevaporated to dryness under reduced pressure
  7. customto afford a white solid

出典と根拠

ORDレコード
ord-14a32d15285245cc88b0fdf6fbdb98ff
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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