Ethyl 2-chloroacetoacetate → HCID 14500742, 화합물

HRID 2350898노트

반응식

HRID 2350898 반응식
[N:1]1([C:7]([NH:9][NH2:10])=S)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[Cl:11][CH:12]([C:18]([CH3:20])=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14]>C(O)C>[ClH:11].[CH3:20][C:18]1[NH:10][N:9]=[C:7]([N:1]2[CH2:6][CH2:5][O:4][CH2:3][CH2:2]2)[C:12]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14]

참가 물질

4

반응물 2

HCID 11858Ethyl 2-chloroacetoacetateHCID 4860905morpholine-4-carbothiohydrazide

생성물 1

HCID 14500742HCID 14500742, 화합물수율 51.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A stirred slurry of 6.3 g (0.039 mole) of 4-morpholinecarbothioic acid hydrazide in 75 mL of absolute ethanol under nitrogen atmosphere was treated with 6.43 g (0.039 mole) of ethyl 2-chloroacetoacetate and the exothermic reaction mixture stirred at ambient temperature for 18 hr. The major portion of reaction mixture solids were dissolved by heating to reflux, the sulfur residue removed by filtration and the filtrate concentrated in vacuo to a solid, which was crystallized from 2-propyl alcohol to yield 5.5 g of white crystalline needles, mp 165°-173° C., as the hydrochloride salt.

후처리

  1. customThe major portion of reaction mixture solids
  2. dissolutionwere dissolved
  3. temperatureby heating
  4. temperatureto reflux
  5. customthe sulfur residue removed by filtration
  6. concentrationthe filtrate concentrated in vacuo to a solid, which
  7. customwas crystallized from 2-propyl alcohol

출처 및 근거

ORD 기록
ord-e729fa25a58c45d9a351c44d0672c07f
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04871737

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