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Hydrazine → HCID 178434214、化合物

HRID 2367480
ノート
印刷プレビュー

反応式

HRID 2367480 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:15]=[C:14]([NH2:16])[N:13]=[C:12]([N:17]3[C@H:22]([CH3:23])[CH2:21][CH2:20][C@H:19]([C:24]([NH:26][CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)=[O:25])[CH2:18]3)[CH:11]=2)=[CH:6][C:5]=1F)(=O)[CH3:2].Cl.CON.C([O-])([O-])=O.[K+].[K+].CCN(C(C)C)C(C)C.[NH2:54][NH2:55]>COCCOC.CCO>[NH2:16][C:14]1[N:13]=[C:12]([N:17]2[C@H:22]([CH3:23])[CH2:21][CH2:20][C@H:19]([C:24]([NH:26][CH2:27][C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=3)=[O:25])[CH2:18]2)[CH:11]=[C:10]([C:7]2[CH:6]=[C:5]3[C:4]([C:1]([CH3:2])=[N:54][NH:55]3)=[CH:9][CH:8]=2)[N:15]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 9321HydrazineHCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 58504436(3S,6R)-1-[6-(4-Acetyl-3-fluorophenyl)-2-amino-4-pyrimidinyl]-6-methyl-N-(phenylmethyl)-3-piperidinecarboxamide

生成物 1

HCID 178434214HCID 178434214、化合物
収率 10.1%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
120 °C

実験手順

Into a sealed tube, (3S,6R)-1-[6-(4-acetyl-3-fluorophenyl)-2-amino-4-pyrimidinyl]-6-methyl-N-(phenylmethyl)-3-piperidinecarboxamide (90 mg, 0.195 mmol), O-methylhydroxylamine hydrochloride (16.3 mg, 0.20 mmol), and K2CO3 (32.3 mg, 0.234 mmol) were stirred together in DME (3 mL) for 4 hours at 57° C. The reaction mixture was filtered, and the filtrate containing the oxime intermediate was concentrated in vacuo to 2 mL. Then EtOH (3 mL), Hunig's base (0.05 mL, 0.27 mmol), and hydrazine anhydrous (0.013 mL, 0.410 mmol) were added, and the resulting yellow mixture was heated overnight at 120° C. in an oil bath. The solution turned black. LCMS showed mainly product. The black solid was filtered and the yellow filtrate was evaporated. The resulting yellow residue was dissolved in CH3OH, and purified by HPLC (CH3CN/H2O w/0.1% HCO2H) to afford a formic acid salt of the title compound (9 mg) as a light yellow solid. LC-MS (ES) m/z=456 [M+H]+. 1H NMR (400 MHz, CD3OD): δ 1.32 (m, 4H), 1.75-1.91 (m, 3H), 1.97-2.12 (m, 1H), 2.41-2.53 (m, 1H), 2.60 (s, 3H), 3.11-3.27 (m, 1H), 4.33-4.50 (m, 2H), 4.56-4.74 (m, 1H), 6.59 (s, 1H), 7.23-7.41 (m, 5H), 7.54-7.63 (m, 1H), 7.96 (m, 1H), 7.94 (s, 1H).

後処理

  1. filtrationThe reaction mixture was filtered
  2. additionthe filtrate containing the oxime intermediate
  3. concentrationwas concentrated in vacuo to 2 mL
  4. filtrationThe black solid was filtered
  5. customthe yellow filtrate was evaporated
  6. dissolutionThe resulting yellow residue was dissolved in CH3OH
  7. custompurified by HPLC (CH3CN/H2O w/0.1% HCO2H)

出典と根拠

ORDレコード
ord-62ac067d1f7748aa89b22baa3f87345f
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697685B2

反応ノート

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