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1,2-Dichloroethane → HCID 41507106、化合物

HRID 1522376
ノート
印刷プレビュー

反応式

HRID 1522376 の反応式
[CH3:1][CH:2]([N:4]1[C:8]2[N:9]=[C:10]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:11]=[C:12]([C:13]([OH:15])=O)[C:7]=2[CH:6]=[N:5]1)[CH3:3].[NH2:22][CH2:23][C:24]1[C:25](=[O:32])[NH:26][C:27]([CH3:31])=[CH:28][C:29]=1[CH3:30].Cl.ON1C2N=CC=CC=2N=N1.CN1CCOCC1.C(Cl)CCl>CS(C)=O.O>[CH3:30][C:29]1[CH:28]=[C:27]([CH3:31])[NH:26][C:25](=[O:32])[C:24]=1[CH2:23][NH:22][C:13]([C:12]1[C:7]2[CH:6]=[N:5][N:4]([CH:2]([CH3:3])[CH3:1])[C:8]=2[N:9]=[C:10]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:11]=1)=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 111,2-DichloroethaneHCID 313Hydrochloric AcidHCID 79724-MethylmorpholineHCID 181649HOAtHCID 25350536-phenyl-1-(propan-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carboxylic acidHCID 70638443-(Aminomethyl)-4,6-dimethyl-1,2-dihydropyridin-2-one

生成物 1

HCID 41507106
HCID 41507106、化合物
収率 70%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

In a 25 mL sealable tube under nitrogen were combined 1-(1-methylethyl)-6-phenyl-1H-pyrazolo[3,4-b]pyridine-4-carboxylic acid (70 mg, 0.25 mmol) and 3-(aminomethyl)-4,6-dimethyl-2(1H)-pyridinone.HCl (56.3 mg, 0.3 mmol) in DMSO (3 mL). 1-hydroxy-7-azabenzotriazole (51 mg, 0.37 mmol) was added and the resulting mixture was degassed with nitrogen for 10 min. N-methylmorpholine (0.1 ml, 0.87 mmol) and EDC (72 mg, 0.37 mmol) were added, the vessel was sealed, and the bright yellow mixture was stirred at room temperature for 2 days. Next added 2 mL of water, and the contents were stirred for 10 min. Solids that precipitated were sonicated, and allowed to stand at room temperature for 10 min. The reaction contents were filtered and washed with water. The solid was treated with 2 mL of EtOH, sonicated and heated, and then allowed to cool to room temperature. The contents were filtered, washed with water and dried to afford the title compound (74 mg, 70%) as a white solid. LCMS E-S (M+H)=416.3. 1H NMR (400 MHz, DMSO-d6) δ ppm 11.58 (s, 1 H), 8.98 (t, J=4.80 Hz, 1 H), 8.38 (s, 1 H), 8.25-8.30 (m, 2 H), 8.17 (s, 1 H), 7.49-7.59 (m, 3 H), 5.91 (s, 1 H), 5.30-5.38 (m, 1 H), 4.42 (d, J=4.80 Hz, 2 H), 2.23 (s, 3 H), 2.13 (s, 3 H), 1.55 (d, J=6.57 Hz, 6 H).

後処理

  1. customIn a 25 mL sealable tube under nitrogen were combined
  2. customthe resulting mixture was degassed with nitrogen for 10 min
  3. customthe vessel was sealed
  4. stirringthe contents were stirred for 10 min
  5. customSolids that precipitated
  6. customwere sonicated
  7. waitto stand at room temperature for 10 min
  8. customThe reaction contents
  9. filtrationwere filtered
  10. washwashed with water
  11. additionThe solid was treated with 2 mL of EtOH
  12. customsonicated
  13. temperatureheated
  14. temperatureto cool to room temperature
  15. filtrationThe contents were filtered
  16. washwashed with water
  17. customdried

出典と根拠

ORDレコード
ord-603b184fa1f64ceab7f16f221c2e6145
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09073924B2

反応ノート

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