2-(4-Bromo-3-oxobutyl)-1H-isoindole-1,3(2H)-dione → HCID 70044281, 화합물

HRID 464635

반응식

HRID 464635 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[C:13]([C:14]([O:16][CH3:17])=[O:15])=[C:12]([CH3:18])[NH:11][C:10]([CH2:19][O:20][CH2:21][C:22]([NH2:24])=[S:23])=[C:9]1[C:25]([O:27][CH2:28][CH3:29])=[O:26].Br[CH2:31][C:32](=O)[CH2:33][CH2:34][N:35]1[C:39](=[O:40])[C:38]2=[CH:41][CH:42]=[CH:43][CH:44]=[C:37]2[C:36]1=[O:45]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[C:13]([C:14]([O:16][CH3:17])=[O:15])=[C:12]([CH3:18])[NH:11][C:10]([CH2:19][O:20][CH2:21][C:22]2[S:23][CH:31]=[C:32]([CH2:33][CH2:34][N:35]3[C:39](=[O:40])[C:38]4=[CH:41][CH:42]=[CH:43][CH:44]=[C:37]4[C:36]3=[O:45])[N:24]=2)=[C:9]1[C:25]([O:27][CH2:28][CH3:29])=[O:26]

참가 물질

4

반응물 2

HCID 37597442-(4-Bromo-3-oxobutyl)-1H-isoindole-1,3(2H)-dioneHCID 13457228HCID 13457228, 화합물

생성물 1

HCID 70044281HCID 70044281, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}thioacetamide (2.19 g) and 1-bromo-4-phthalimido-2-butanone (1.48 g) in ethanol (50 ml) was heated under reflux for 4 hours and then evaporated. The residue was triturated with ether/hexane and the resulting solid collected, recrystallised from methanol and dried to give 2-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxymethyl}-4-(2-phthalimidoethyl)thiazole as a hemihydrate (1.73 g), m.p. 156°-157° C. Found: C,59.71; H,5.06; N,6.31. C32H29ClN3O7S.0.5H2O: requires C,59.58; H,4.80; N,6.51%.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. customevaporated
  4. customThe residue was triturated with ether/hexane
  5. customthe resulting solid collected
  6. customrecrystallised from methanol
  7. customdried

출처 및 근거

ORD 기록
ord-b935ca7ad26b4904a13bbcdcb2be0842
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04548935

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