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Water → HCID 57865098、化合物

HRID 886664
ノート
印刷プレビュー

反応式

HRID 886664 の反応式
N1N[N:3]=[N:4][C:5]=1[C:6]1[CH:7]=[N:8][C:9]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2.[N:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[C:22](Cl)(=[O:32])[C:23]1[CH:31]=[CH:30][CH:29]=[C:25]([C:26](Cl)=[O:27])[CH:24]=1.O>CCCCCC.C(Cl)(Cl)Cl>[N:16]1[C:21]2[C:20](=[CH:7][CH:6]=[CH:15][CH:14]=2)[CH:19]=[C:18]([C:5]2[O:32][C:22]([C:23]3[CH:31]=[CH:30][CH:29]=[C:25]([C:26]4[O:27][C:5]([C:6]5[CH:7]=[N:8][C:9]6[C:14]([CH:15]=5)=[CH:13][CH:12]=[CH:11][CH:10]=6)=[N:4][N:3]=4)[CH:24]=3)=[N:3][N:4]=2)[CH:17]=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

7

反応物 4

HCID 962WaterHCID 1049PyridineHCID 7451Isophthaloyl chlorideHCID 223956903-(2H-Tetrazol-5-yl)quinoline

生成物 1

HCID 57865098HCID 57865098、化合物収率 82%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒
HCID 8058
Hexane
溶媒

反応条件

温度
100 °C

実験手順

After dissolving 4.0 g of 3-(2H-tetrazole-5-yl)-quinoline into 60 ml of dehydrated pyridine, 2.1 g of isophthaloylchloride was added. The mixture was heated to 100° C. and stirred under reflux for 3 hours. After cooling to a room temperature, the reaction solution was poured into water to collect a precipitated solid by suction filtration, and the solid was washed with water. The solid was dried under vacuum at 70° C. for 20 hours to obtain a grayish white crude product. After dissolving the thus-obtained crude product into chloroform, hexane was added to allow purification by crystallization, thereby obtaining 3.90 g of 3QOXDm (31) (yield: 82%). NMR analysis (see FIG. 4) was performed for identification of the product. The results of the NMR analysis are as follows. 9.70 ppm (2H), 9.02 ppm (1H), 8.98 ppm (2H), 8.46 ppm (2H), 8.24 ppm (2H), 8.05 ppm (2H), 7.89 ppm (2H), 7.83 ppm (1H), 7.71 ppm (2H).

後処理

  1. additionwas added
  2. temperatureunder reflux for 3 hours
  3. temperatureAfter cooling to a room temperature
  4. customto collect a precipitated solid
  5. filtrationby suction filtration
  6. washthe solid was washed with water
  7. customThe solid was dried under vacuum at 70° C. for 20 hours
  8. customto obtain a grayish white crude product
  9. dissolutionAfter dissolving the
  10. additionwas added
  11. custompurification
  12. customby crystallization

出典と根拠

ORDレコード
ord-6991daa86be0470caf72a6a45e4099a5
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08247087B2

反応ノート

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