Ethyl 2-chloroacetoacetate → HCID 14500742、化合物

HRID 1761558ノート

反応式

HRID 1761558 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 14500742HCID 14500742、化合物収率 51.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d9a4da3eacb24090900e54afef2db407
出典データセット
uspto-grants-1989_05
特許番号
US04826866

反応ノート

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