Salicylamide → 8-[(2-Hydroxybenzoyl)aminomethyl]-2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione

HRID 1381949노트

반응식

HRID 1381949 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:16]([NH2:25])(=[O:24])[C:17]1[C:18](=[CH:20][CH:21]=[CH:22][CH:23]=1)[OH:19].[CH2:26](N(CC)CC)C>C(O)C>[OH:19][C:18]1[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=1[C:16]([NH:25][CH2:26][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:24]

참가 물질

5

반응물 3

HCID 5147SalicylamideHCID 8471TriethylamineHCID 30882852,8-Diazaspiro(4,5)decane-1,3-dione, 2-methoxy-, monohydrochloride

생성물 1

HCID 143718678-[(2-Hydroxybenzoyl)aminomethyl]-2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A suspension of 2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione.hydrochloride (0.55 g), salicylamide (0.32 g), p-formaldehyde (0.11 g) and triethylamine (2 ml) in ethanol (20 ml) was stirred for 15 hours at room temperature. Then, the solvent was evaporated off under reduced pressure, and the residual oily product was subjected to a silica gel column chromatography (eluent; ethyl acetate), and the solvent for the solution containing the desired product was evaporated off under reduced pressure. The residual solid was recrystallized from ethyl ether to obtain 0.52 g of colorless crystals, m.p. 96° to 99° C.

후처리

  1. customThen, the solvent was evaporated off under reduced pressure
  2. additionthe solvent for the solution containing the desired product
  3. customwas evaporated off under reduced pressure
  4. customThe residual solid was recrystallized from ethyl ether

출처 및 근거

ORD 기록
ord-3e3ea5c82e6b43b683e01ef68c0d40c1
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804665

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