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

HRID 1381944노트

반응식

HRID 1381944 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8be582bcf9b94aa4a71bbee6cb454af0
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804665

반응 노트

불러오는 중…