Hydrochloric Acid → HCID 178468491、化合物

HRID 1879922ノート

反応式

HRID 1879922 の反応式
Cl[C:2]1[N:11]=[C:10]([OH:12])[C:9]2[C:4](=[CH:5][C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1.[CH2:17]([O:19][C:20]([C:22]1([CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)=[O:21])[CH3:18].Cl.CCN(C(C)C)C(C)C>C(O)C>[CH2:17]([O:19][C:20]([C:22]1([CH2:28][C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH2:23][CH2:24][N:25]([C:2]2[N:11]=[C:10]([OH:12])[C:9]3[C:4](=[CH:5][C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=3)[N:3]=2)[CH2:26][CH2:27]1)=[O:21])[CH3:18]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 53297794Ethyl 4-benzylpiperidine-4-carboxylateHCID 178486816HCID 178486816、化合物

生成物 1

HCID 178468491HCID 178468491、化合物収率 87%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1.2 g (5 mmol) 2-Chloro-6,7-dimethoxy-quinazolin-4-ol (commercially available), 2.26 g (8 mmol) 4-Benzyl-piperidine-4-carboxylic acid ethyl ester; hydrochloride and 1.93 g (15 mmol) DIPEA in 80 mL ethanol was heated to reflux for 62 h. The mixture was concentrated, the precipitate filtered off and washed with ethanol and diethyl ether. The residue was dried. 1.9 g (87%) of the title compound was isolated as white solid. MS (m/e): 452.2 (MH+).

後処理

  1. temperatureto reflux for 62 h
  2. concentrationThe mixture was concentrated
  3. filtrationthe precipitate filtered off
  4. washwashed with ethanol and diethyl ether
  5. customThe residue was dried

出典と根拠

ORDレコード
ord-aa5c635bbc684f72bb11a0fa9105a0d8
出典データセット
uspto-grants-2012_11
特許番号
US08318749B2

反応ノート

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