Methanol → 5-[5-(N-acetyl-anilino)-2, 3-pentadienylidene]-2,7-diphenyl-4-methylpyrazolo[3,4-b]pyridine-3,6-dione

HRID 1073047

反応式

HRID 1073047 の反応式
CO.[C:3]1([N:9]2[C:17](=[O:18])[C:16]3[C:15]([CH3:19])=[CH:14][C:13](=[O:20])[N:12]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[C:11]=3[NH:10]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl.C1(N=[CH:35][CH:36]=[CH:37][CH:38]=[CH:39][NH:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)C=CC=CC=1.[C:47](OC(=O)C)(=[O:49])[CH3:48]>C(N(CC)CC)C>[C:47]([N:40]([CH2:39][CH:38]=[C:37]=[CH:36][CH:35]=[C:14]1[C:13](=[O:20])[N:12]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:11]2=[N:10][N:9]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=3)[C:17](=[O:18])[C:16]2=[C:15]1[CH3:19])[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1)(=[O:49])[CH3:48]

参加物

6

反応物 4

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 73902N-(5-(phenylamino)penta-2,5-dienylidene)aniline monohydrochlorideHCID 3603164-methyl-2,7-diphenyl-1H-pyrazolo[3,4-b]pyridine-3,6-dione

生成物 1

HCID 571236985-[5-(N-acetyl-anilino)-2, 3-pentadienylidene]-2,7-diphenyl-4-methylpyrazolo[3,4-b]pyridine-3,6-dione

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

In a solution prepared by adding methanol (50 ml) and triethylamine (2.8 ml) to 2,7-diphenyl-4-methylpyrazolo(3,4-b) pyridine-3,6-dione (3.17 g), 1,7-diphenyl-1,7-diaza-1,3,5-heptatriene hydrochloride (2.85 g) was dissolved and then acetic anhydride (1.88 ml) was added, and the mixture was stirred at room temperature for one hour. The resulting precipitate was collected by filtration, washed with methanol and dried to obtain 5-[5-(N-acetylanilino)-2,3-pentadienylidene]-2,7-diphenyl-4-methylpyrazolo(3,4-b)pyridin-3, 6-dione (1.9). To these crystals (1.5 g), N,N-dimethylformamide (60 ml), 2,7-diphenyl-4-methylpyrazolo(3,4-b)pyridin-3,6-dione (0.95 g) and triethylamine (0.42 g) were added, and stirred at 50° C. for 2 hours. After a trace amount of insoluble matters were removed by filtration, ethyl acetate of 10-fold the volume of the filtrate was added thereto while stirring for crystallization. The resulting crystals were redissolved in a small amount of N,N-dimethylformamide, and a 10-fold volume of ethyl acetate was added thereto for crystallization. The resulting crystals were collected by filtration and dried to obtain compound II-2 (1.3 g). Gold crystals, melting point 300° C. or more, λmaxDMF 792 nm

後処理

  1. customIn a solution prepared
  2. dissolutionwas dissolved
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with methanol
  5. customdried

出典と根拠

ORDレコード
ord-5d4fb42d68014090b545eac1426edc4c
出典データセット
uspto-grants-1990_11
特許番号
US04968593

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