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Ammonium Chloride → HCID 86677324、化合物

HRID 1842669
ノート
印刷プレビュー

反応式

HRID 1842669 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[CH2:10][CH2:11][N:12]([CH3:15])[CH2:13][CH:14]=2)[C:6]([N+:16]([O-])=O)=[CH:5][C:4]=1[NH:19][C:20]1[N:25]=[C:24]([C:26]2[CH:27]=[N:28][N:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=23)[C:23]([CH3:35])=[CH:22][N:21]=1.[NH4+].[Cl-]>C(O)C.O.[Fe]>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[CH2:10][CH2:11][N:12]([CH3:15])[CH2:13][CH:14]=2)[C:6]([NH2:16])=[CH:5][C:4]=1[NH:19][C:20]1[N:25]=[C:24]([C:26]2[CH:27]=[N:28][N:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=23)[C:23]([CH3:35])=[CH:22][N:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 25517Ammonium Chloride2 回HCID 71240803HCID 71240803、化合物2 回

生成物 1

HCID 86677324HCID 86677324、化合物収率 57.6%

試薬・触媒・溶媒 3

HCID 23925Iron触媒2 回HCID 702Ethanol溶媒HCID 962Water
溶媒

実験手順

A mixture of N-[2-methoxy-4-(1-methyl-3,6-dihydro-2H-pyridin-4-yl)-5-nitrophenyl]-5-methyl-4-pyrazolo[1,5-a]pyridin-3-ylpyrimidin-2-amine (Intermediate 2, 279 mg, 0.59 mmol), iron (198 mg, 3.55 mmol) and NH4Cl (22.16 mg, 0.41 mmol) in ethanol (10.5 mL) and water (3.50 mL) was heated at reflux for 0.75 h. Further NH4Cl (22.16 mg, 0.41 mmol) and iron (198 mg, 3.55 mmol) were then added and the mixture was heated at reflux for a further 1.5 h. The mixture was then cooled, filtered, and the filtrate was concentrated in vacuo. Purification by FCC, eluting with 2-10% 7N methanolic ammonia in CH2Cl2 gave the title compound (150 mg, 57%) as a beige crystalline solid after trituration with THF and washing the resulting solid with diethyl ether; 1H NMR: 2.30 (3H, s), 2.40 (5H, m), 2.59 (2H, t), 3.01 (2H, d), 3.73 (3H, s), 4.27 (2H, s), 5.71 (1H, s), 6.63 (1H, s), 7.10 (1H, m), 7.35-7.49 (2H, m), 7.83 (1H, s), 8.27 (1H, s), 8.50-8.63 (2H, m), 8.81 (1H, d); m/z: ES+ MH+ 442.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 0.75 h
  3. temperaturethe mixture was heated
  4. temperatureat reflux for a further 1.5 h
  5. temperatureThe mixture was then cooled
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated in vacuo
  8. customPurification by FCC
  9. washeluting with 2-10% 7N methanolic ammonia in CH2Cl2

出典と根拠

ORDレコード
ord-d0085a99c57a43668fdb136c80b35075
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946235B2

反応ノート

読み込み中…

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