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Triethylamine → 4-Oxo-N-((4'-((((5-oxo-4,5-dihydro-1H-1,2,4-triazol-3-yl)methyl)sulfonyl)methyl)biphenyl-3-yl)methyl)-3,4-dihydroquinazoline-2-carboxamide

HRID 606433
ノート
印刷プレビュー

反応式

HRID 606433 の反応式
[NH2:1][CH2:2][C:3]1[CH:4]=[C:5]([C:9]2[CH:14]=[CH:13][C:12]([CH2:15][S:16]([CH2:19][C:20]3[NH:21][C:22](=[O:25])[NH:23][N:24]=3)(=[O:18])=[O:17])=[CH:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1.[O:26]=[C:27]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[N:30]=[C:29]([C:37](OCC)=[O:38])[NH:28]1.C(N(CC)CC)C.CC(N(C)C)=O>CCO.C(OCC)(=O)C>[O:26]=[C:27]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[N:30]=[C:29]([C:37]([NH:1][CH2:2][C:3]2[CH:4]=[C:5]([C:9]3[CH:14]=[CH:13][C:12]([CH2:15][S:16]([CH2:19][C:20]4[NH:21][C:22](=[O:25])[NH:23][N:24]=4)(=[O:17])=[O:18])=[CH:11][CH:10]=3)[CH:6]=[CH:7][CH:8]=2)=[O:38])[NH:28]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 31374DimethylacetamideHCID 135437466Ethyl 4-oxo-3,4-dihydroquinazoline-2-carboxylateHCID 1360544705-[({[3'-(aminomethyl)biphenyl-4-yl]methyl}sulfonyl)methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

生成物 1

HCID 1360544874-Oxo-N-((4'-((((5-oxo-4,5-dihydro-1H-1,2,4-triazol-3-yl)methyl)sulfonyl)methyl)biphenyl-3-yl)methyl)-3,4-dihydroquinazoline-2-carboxamide
収率 55%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 5-[({[3′-(aminomethyl)biphenyl-4-yl]methyl}sulfonyl)methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one obtained in Reference Example 111 (0.060 g, 0.167 mmol), ethyl 4-oxo-3,4-dihydro-2-quinazolinecarboxylate obtained according to the methods described in Journal of Organic Chemistry (1978), 43(23), 4485-7 and the like (0.024 g, 0.112 mmol) and triethylamine (0.389 mL, 1.12 mmol) in EtOH (3 mL)-DMA (3 mL) was stirred at 90° C. for 24 hr. The reaction mixture was diluted with ethyl acetate, washed with 0.1N hydrochloric acid and saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from EtOH-diethyl ether to give the title compound as a pale-yellow powder (0.032 g, 55%).

後処理

  1. customobtained
  2. washwashed with 0.1N hydrochloric acid and saturated brine
  3. dry with materialdried over sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was crystallized from EtOH-diethyl ether

出典と根拠

ORDレコード
ord-2344f62c362b4664ba4ddf5775acdd18
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915267B2

反応ノート

読み込み中…

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