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Potassium Carbonate → HCID 178432267、化合物

HRID 2254123
ノート
印刷プレビュー

反応式

HRID 2254123 の反応式
Cl[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]=[C:4]([CH3:12])[N:3]=1.Cl.[NH:14]1[C:18]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[C:25]2[CH:30]=[CH:29][C:28]([CH2:31][NH2:32])=[CH:27][CH:26]=2)=[N:17][N:16]=[N:15]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[NH:17]1[C:18]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[C:25]2[CH:30]=[CH:29][C:28]([CH2:31][NH:32][C:2]3[C:11]4[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=4[N:5]=[C:4]([CH3:12])[N:3]=3)=[CH:27][CH:26]=2)=[N:14][N:15]=[N:16]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

5

反応物 3

HCID 11430Potassium CarbonateHCID 197442074-Chloro-2-methyl-5,6,7,8-tetrahydroquinazolineHCID 178479176(4-(2-(1H-1,2,3,4-tetrazol-5-yl)phenyl)phenyl)methanamine hydrochloride

生成物 1

HCID 178432267HCID 178432267、化合物収率 31%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
95 °C

実験手順

To 10 mL of dimethylformamide were added 0.57 g of 4-chloro-5,6,7,8-tetrahydro-2-methylquinazoline, 0.45 g of N-[[2'-(1H-tetrazol-5-yl)[1,1'-biphenyl]-4-yl]methyl]amine hydrochloride and 1.30 g of anhydrous potassium carbonate. The resulting mixture was heated at 95° C. for 5 days and then cooled to room temperature. The resulting mixture was run through a silica plug (methanol/chloroform/ammonia eluant) and after all solvent was removed by evaporation the resulting residue was purified on silica to yield 0.19 g (31%) of the desired product. The compound was characterized as its potassium salt: 1H NMR (DMSO-d6, 400 MHz) δ 7.50 (m, 1H), 7.32 (m, 3H), 7.11 (d, J=8.2 HZ, 2H), 7.02 (m, 3H), 4.57 (d, J=6.0 Hz, 2H), 2.48 (m, 4H);, 2.24 (s, 3H), 1.71 (m, 4H); negative FAB-MS m/e 433(M-H); 396(M-K). Anal. calcd for C23H22KN7.0.85H2O: C, 61.53; H, 5.30; N, 21.84. Found: C, 61.74; H, 5.25; N, 21.47.

後処理

  1. temperaturecooled to room temperature
  2. customafter all solvent was removed by evaporation the resulting residue
  3. customwas purified on silica

出典と根拠

ORDレコード
ord-721b1e4f9afe447b918296985ddbe15a
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05234936

反応ノート

読み込み中…

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