Ethyl 2-chloroacetoacetate → HCID 178432410、化合物

HRID 477222

反応式

HRID 477222 の反応式
[NH2:1][C:2]1[N:6]=[C:5]([S:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[NH:4][N:3]=1.[Cl:15][CH:16]([C:22]([CH3:24])=O)[C:17](OCC)=[O:18]>C(O)(=O)C>[CH2:8]([S:7][C:5]1[N:6]=[C:2]2[N:1]=[C:22]([CH3:24])[C:16]([Cl:15])=[C:17]([OH:18])[N:3]2[N:4]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 11858Ethyl 2-chloroacetoacetateHCID 178509291HCID 178509291、化合物

生成物 1

HCID 178432410HCID 178432410、化合物収率 60%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 16 g (77 mmol) of 3-amino-5-benzylthio-1,2,4-triazole and 10.6 g (77 mmol) of ethyl 2-chloroacetoacetate in 150 ml of glacial acetic acid was heated at 100° C. for 17 hours. Upon cooling to room temperature the solid which separated was collected by filtration. The filtrate was diluted with ice water to separate an additional quantity of solid. The solids were combined and dried to yield 14.0 g (60% of the desired product as a solid, m.p. 258°-260° C. IR and 1H NMR were in agreement with the assigned structure.

後処理

  1. customseparated
  2. filtrationwas collected by filtration
  3. additionThe filtrate was diluted with ice water
  4. customto separate an additional quantity of solid
  5. customdried

出典と根拠

ORDレコード
ord-11643bfd920c48288a6c4f28df5dc2d5
出典データセット
uspto-grants-1989_12
特許番号
US04886883

関連ノート

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