Acryloyl chloride → HCID 178460006、化合物

HRID 370704

反応式

HRID 370704 の反応式
Cl.Cl.[NH2:3][C:4]1[CH:12]=[CH:11][C:7]2[NH:8][N:9]=[N:10][C:6]=2[CH:5]=1.C(=O)([O-])O.[Na+].[C:18](Cl)([CH:20]=[CH2:21])=[O:19]>O>[C:18]([NH:3][C:4]1[CH:12]=[CH:11][C:7]2[NH:8][N:9]=[N:10][C:6]=2[CH:5]=1)(=[O:19])[CH:20]=[CH2:21]

参加物

5

反応物 3

HCID 13140Acryloyl chlorideHCID 516892Sodium BicarbonateHCID 178478652HCID 178478652、化合物

生成物 1

HCID 178460006HCID 178460006、化合物収率 58.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

20.7 g of 5-aminobenzotriazole dihydrochloride and 30 g of sodium hydrogen carbonate were dissolved in 300 ml of water, and 10 g of acryl chloride was added dropwise at a temperature of lower than 10° C. over 20 minutes. After being stirred for 1 hour, the formed white precipitate was filtered off. Yield: 13.8 g. It was dissolved in 100 ml of DMF, and 500 ml of hot water at about 70° C. was added. It was immediately filtered under atmospheric pressure. The filtrate was allowed to cool, and the separated crystals were filtered out, washed with water and dried to obtain 11 g of the desired product which melted at 248°-253° C. The structure was confirmed by IR, NMR and elementary analysis.

後処理

  1. filtrationthe formed white precipitate was filtered off
  2. dissolutionIt was dissolved in 100 ml of DMF
  3. addition500 ml of hot water at about 70° C. was added
  4. filtrationIt was immediately filtered under atmospheric pressure
  5. temperatureto cool
  6. filtrationthe separated crystals were filtered out
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-fd874fcb90364f05b78097c74f8e01c8
出典データセット
uspto-grants-1985_07
特許番号
US04528264

関連ノート

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