Tetrahydrofuran → 4-(3-Ethoxycarbonylpropyl)Amino-6,7,8-Trimethoxyquinazoline

HRID 1603524

반응식

HRID 1603524 반응식
Cl.[NH2:2][CH2:3][CH2:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].C(N(CC)CC)C.O1CCCC1.Cl[C:24]1[C:33]2[C:28](=[C:29]([O:38][CH3:39])[C:30]([O:36][CH3:37])=[C:31]([O:34][CH3:35])[CH:32]=2)[N:27]=[CH:26][N:25]=1>CC(O)C>[CH2:9]([O:8][C:6]([CH2:5][CH2:4][CH2:3][NH:2][C:24]1[C:33]2[C:28](=[C:29]([O:38][CH3:39])[C:30]([O:36][CH3:37])=[C:31]([O:34][CH3:35])[CH:32]=2)[N:27]=[CH:26][N:25]=1)=[O:7])[CH3:10]

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 1006864-Chloro-6,7,8-trimethoxyquinazolineHCID 126496614-Aminobutyrate ethyl hydrochloride

생성물 1

HCID 97984504-(3-Ethoxycarbonylpropyl)Amino-6,7,8-Trimethoxyquinazoline수율 72%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

1.0 g of ethyl 4-aminobutyrate hydrochloride (6.0 mmol), 2 ml of triethylamine, 10 ml of tetrahydrofuran and 10 ml of 2-propanol are added to 0.50 g (2.0 mmol) of 4-chloro-6,7,8-trimethoxyquinazoline, followed by heating under reflux one whole day and night. The reaction liquid is distilled under reduced pressure to remove the solvent. The obtained residue is purified by silica gel column chromatography (ethyl acetate) and then recrystallized from ethyl acetate/hexane. Thus, 0.49 g (yield 72%) of a white crystal is obtained.

후처리

  1. temperatureby heating
  2. temperatureunder reflux one whole day and night
  3. customThe reaction liquid
  4. distillationis distilled under reduced pressure
  5. customto remove the solvent
  6. customThe obtained residue is purified by silica gel column chromatography (ethyl acetate)
  7. customrecrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-f89c6bd37f1e46618a85f45d67f39c63
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990117

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