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Acetic Acid → HCID 178480125、化合物

HRID 605000
ノート
印刷プレビュー

反応式

HRID 605000 の反応式
Cl.Cl.[NH:3]1[CH2:8][CH2:7][CH:6]([C:9]2[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[NH:11][N:10]=2)[CH2:5][CH2:4]1.[CH3:20][N:21]1[CH:30]=[CH:29][C:28]2[N:27]=[C:26]([C:31]3[CH:38]=[CH:37][C:34]([CH:35]=O)=[CH:33][CH:32]=3)[C:25]([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)=[CH:24][C:23]=2[C:22]1=[O:45].C(N(CC)CC)C.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>CN(C=O)C>[CH3:20][N:21]1[CH:30]=[CH:29][C:28]2[N:27]=[C:26]([C:31]3[CH:38]=[CH:37][C:34]([CH2:35][N:3]4[CH2:8][CH2:7][CH:6]([C:9]5[N:13]=[C:12]([C:14]6[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=6)[NH:11][N:10]=5)[CH2:5][CH2:4]4)=[CH:33][CH:32]=3)[C:25]([C:39]3[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=3)=[CH:24][C:23]=2[C:22]1=[O:45]
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 8471TriethylamineHCID 5049666Sodium triacetoxyborohydride2 回HCID 866249424-(6-Methyl-5-oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehydeHCID 1784785342-(5-Piperidin-4-yl-4h-1,2,4-triazol-3-yl)-pyridine dihydrochloride

生成物 1

HCID 178480125
HCID 178480125、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-(3-piperidin-4-yl-1H-1,2,4-triazol-5-yl)pyridine dihydrochloride (142 mg, 10.47 mmol) and 4-(6-methyl-5-oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehyde (5141 mg, 0.415 mmol) in dry DMF (1.5 mL) was added triethylamine (0.21 mL, 1.5 mmol). After stirring for 10 minutes acetic acid (0.26 mL, 4.5 mmol) was added and the mixture was stirred at room temperature over night. Then sodium triacetoxy borohydride (110 mg, 0.52 mmol) was added in one portion and stirred for eight hours. After monitoring by LC/MS determined the reaction was not complete additional sodium triacetoxy borohydride (46 mg, 0.21 mmol)) were added and the reaction was stirred over night. This reaction mixture was adsorbed on silica gel and purified by column chromatography eluting with 1-7% methanol/ethyl acetate (sat'd NH3). The appropriate fractions were combined, the solvents removed in vacuo, and the residue digested in acetonitrile containing a little methanol to give pure title compound. 1H NMR (500 MHz, CDCl3): δ 8.69 (1H, s), 8.65 (1H, d, J=4.4 Hz), 8.15 (1H, d, J=7.8 Hz), 7.83 (1H, t, J=7.6 Hz), 7.31-7.39 (5H, m), 7.22-7.25 (6H, m), 6.86 (1H, d, J=6.5 Hz), 3.66 (3H, s), 3.53 (2H, s), 2.95 (2H, br d, J=10.7 Hz), 2.85 (1H, m), 2.06-2.15 (4H, m), 1.92-2.01 (2H, m). m/e (m+1): 554.3, 277.9 [(m+2)/2].

後処理

  1. additionwas added
  2. stirringstirred for eight hours
  3. additionwere added
  4. stirringthe reaction was stirred over night
  5. custompurified by column chromatography
  6. washeluting with 1-7% methanol/ethyl acetate (sat'd NH3)
  7. customthe solvents removed in vacuo

出典と根拠

ORDレコード
ord-b6b799212b9d43eb82251d43ef42a841
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07910561B2

反応ノート

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