Dichloromethane → 8-Acetyl-2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione

HRID 1381944ノート

反応式

HRID 1381944 の反応式
Cl.[CH3:2][O:3][N:4]1[C:8](=[O:9])[CH2:7][C:6]2([CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[C:5]1=[O:15].C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24].ClCCl>CN(C)C=O>[C:23]([N:12]1[CH2:13][CH2:14][C:6]2([C:5](=[O:15])[N:4]([O:3][CH3:2])[C:8](=[O:9])[CH2:7]2)[CH2:10][CH2:11]1)(=[O:25])[CH3:24]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 30882852,8-Diazaspiro(4,5)decane-1,3-dione, 2-methoxy-, monohydrochloride

生成物 1

HCID 143718338-Acetyl-2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione hydrochloride (2.35 g) in dimethylformamide (200 ml) was added triethylamine (2.8 ml), followed by acetyl chloride (0.8 ml), and this was followed by 30 minutes of stirring at room temperature. To the resulting residual oily substance dichloromethane (50 ml) was added, after which it was washed with 1N hydrochloric acid and then with water. After drying the organic layer with anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure; the resulting residual solid was recrystallized from ethanol-ethyl ether to obtain 1.2 g of a colorless crystal having a melting point of from 153° to 157° C.

後処理

  1. washafter which it was washed with 1N hydrochloric acid
  2. dry with materialAfter drying the organic layer with anhydrous magnesium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customthe resulting residual solid was recrystallized from ethanol-ethyl ether

出典と根拠

ORDレコード
ord-8be582bcf9b94aa4a71bbee6cb454af0
出典データセット
uspto-grants-1989_02
特許番号
US04804665

反応ノート

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