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Methanol → HCID 67995133、化合物

HRID 2361387
ノート
印刷プレビュー

反応式

HRID 2361387 の反応式
Cl[C:2]1[C:7]2[NH:8][C:9]3[CH:10]=[C:11]([C:15](=[O:17])[CH3:16])[CH:12]=[CH:13][C:14]=3[C:6]=2[C:5]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([N+:24]([O-])=O)[C:19]=2[CH3:27])=[N:4][N:3]=1.[CH3:28]O.[C:30]([O-:33])(=[O:32])C.[Na+]>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.[Fe+2].C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CO.C(Cl)Cl>[C:15]([C:11]1[CH:12]=[CH:13][C:14]2[C:6]3[C:5]([C:18]4[CH:23]=[CH:22][CH:21]=[C:20]([NH2:24])[C:19]=4[CH3:27])=[N:4][N:3]=[C:2]([C:30]([O:33][CH3:28])=[O:32])[C:7]=3[NH:8][C:9]=2[CH:10]=1)(=[O:17])[CH3:16]
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

7

反応物 3

HCID 887MethanolHCID 517045Sodium AcetateHCID 86681526HCID 86681526、化合物

生成物 1

HCID 67995133HCID 67995133、化合物収率 60.9%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒HCID 635956
Ferrocene-1,1'-bis-(diphenylphosphine)
触媒
HCID 21226129Dichloromethane methanol溶媒

反応条件

温度
95 °C

実験手順

1-(4-Chloro-1-(2-methyl-3-nitrophenyl)-5H-pyridazino[4,5-b]indol-7-yl)ethanone (0.90 g, 2.364 mmol), methanol (30 mL, 740 mmol), DPPF (0.197 g, 0.355 mmol), palladium (II) acetate (0.080 g, 0.355 mmol), and sodium acetate (0.388 g, 4.73 mmol) were placed into a steel bomb. The bomb was evacuated and refilled with nitrogen. This operation was once repeated. The bomb was vacuumed again and then charged with CO (g) at 50 psi. The bomb was then heated at 95° C. for 20 hr. Upon cooling to room temperature, the bomb was further cooled at −78° C. and the excess CO (g) was released. The reaction mixture was diluted with ethyl acetate (20 mL) and filtered through CELITE®. The filtrate was concentrated under vacuum. The residue was diluted with ethyl acetate (180 mL), washed with water (2×40 mL) and brine (40 mL), and dried over anhydrous. The desired product, methyl 7-acetyl-1-(3-amino-2-methylphenyl)-5H-pyridazino[4,5-b]indole-4-carboxylate (0.539 g, 1.440 mmol, 60.9% yield), was isolated as a beige solid by ISCO (120 g silica gel, 1-5% methanol/CH2Cl2).

後処理

  1. customThe bomb was evacuated
  2. additionrefilled with nitrogen
  3. additioncharged with CO (g) at 50 psi
  4. temperatureUpon cooling to room temperature
  5. temperaturethe bomb was further cooled at −78° C.
  6. additionThe reaction mixture was diluted with ethyl acetate (20 mL)
  7. filtrationfiltered through CELITE®
  8. concentrationThe filtrate was concentrated under vacuum
  9. additionThe residue was diluted with ethyl acetate (180 mL)
  10. washwashed with water (2×40 mL) and brine (40 mL)
  11. customdried over anhydrous

出典と根拠

ORDレコード
ord-1703dc310dce45d69a713800187d1e04
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685969B2

反応ノート

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