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

HRID 1603524ノート

反応式

HRID 1603524 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f89c6bd37f1e46618a85f45d67f39c63
出典データセット
uspto-grants-1999_11
特許番号
US05990117

反応ノート

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