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Acetic Acid → (6-Ethyl-8-phenyl-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl)-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-amine

HRID 2076041
ノート
印刷プレビュー

反応式

HRID 2076041 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([NH:16][C:17]2[N:18]=[CH:19][C:20]3[CH2:26][NH:25][CH2:24][CH:23]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[C:21]=3[N:22]=2)[CH:7]=[CH:8][C:9]=1[N:10]1[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]1.[CH2:33](N)[CH3:34].C(=O)C.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>O1CCCC1>[CH2:33]([N:25]1[CH2:24][CH:23]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[N:22]=[C:17]([NH:16][C:6]3[CH:7]=[CH:8][C:9]([N:10]4[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]4)=[C:4]([O:3][CH3:2])[CH:5]=3)[N:18]=[CH:19][C:20]=2[CH2:26]1)[CH3:34]
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 5

HCID 176Acetic AcidHCID 177AcetaldehydeHCID 6341EthylamineHCID 5049666Sodium triacetoxyborohydrideHCID 44194157[3-Methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-(8-phenyl-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl)-amine hydrochloride

生成物 1

HCID 44194160
(6-Ethyl-8-phenyl-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl)-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-amine
収率 61%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of [3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-(8-phenyl-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl)-amine hydrochloride (75 mg, 0.17 mmol) in tetrahydrofuran (3.3 mL) was added at room temperature NN,-diisoprpyl ethyl amine (43 mg, 0.33 mmol). After stirring for 5 minutes at room temperature acetaldehyde (8.1 mg, 0.18 mmol), acetic acid (20 mg, 0.33 mmol) and sodium triacetoxyborohydride (106 mg, 0.50 mmol) were added. The reaction was stirred at room temperature over night. The solvent was evaporated under reduced pressure and the residue was purified by column chromatography on silica gel using dichloromethane/methanol (95:5 v/v) as eluent to yield the title compound (45 mg, 61%) as a yellow gum. MS ISN (m/e): 439.6 (100) [(M−H)−]. 1H NMR (CDCl3, 300 MHz): δ (ppm)=8.24 (s, 1H), 7.62 (s, 1H), 7.54 (s, 1H), 7.20-7.34 (m, 5H), 7.02 (d, 1H), 6.79 (s, 1H), 6.70 (d, 1H), 4.24 (m, 1H), 3.76 (d, 1H), 3.54 (d, 1H), 3.33 (s, 3H), 3.20 (dd, 1H), 2.60 (m, 3H), 2.67 (s, 3H), 1.17 (t, 3H).

後処理

  1. additionwere added
  2. customThe solvent was evaporated under reduced pressure
  3. customthe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-6a5328c5c57b48d3924b1719214f0485
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07923450B2

反応ノート

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