Ethyl 2-chloroacetoacetate → HCID 178432410, 화합물

HRID 477222

반응식

HRID 477222 반응식
[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

참가 물질

4

반응물 2

HCID 11858Ethyl 2-chloroacetoacetateHCID 178509291HCID 178509291, 화합물

생성물 1

HCID 178432410HCID 178432410, 화합물수율 60%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-11643bfd920c48288a6c4f28df5dc2d5
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886883

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