Hydrochloric Acid → HCID 14500702, 화합물

HRID 1761545노트

반응식

HRID 1761545 반응식
[CH:1]1([NH:7][C:8](=S)[NH:9][NH2:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:12][CH:13]([C:19]([CH3:21])=O)[C:14]([O:16][CH2:17][CH3:18])=[O:15].Cl>C(O)C>[ClH:12].[CH:1]1([NH:7][C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:19]([CH3:21])[NH:10][N:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11858Ethyl 2-chloroacetoacetateHCID 722813Hydrazinecarbothioamide, N-cyclohexyl-

생성물 1

HCID 14500702HCID 14500702, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 34.7 g (0.2 mole) of 4-cyclohexyl-3-thiosemicarbazide and 32.9 g (0.2 mole) of ethyl 2-chloroacetoacetate in 350 mL of absolute ethanol was stirred under nitrogen atmosphere at ambient temperature for 2 hr, treated with 100 mL of 2N ethanolic hydrogen chloride and heated at reflux for 2 hr. The hot reaction mixture was filtered to remove an amorphous solid. The product persistently crystallized in the filter. The product was recrystallized from acetone and recovered by decating off hot acetone solvent and washing the residue with cold acetone to give 27 g of large, off-white crystals, mp 178°-182° C.

후처리

  1. temperatureheated
  2. temperatureat reflux for 2 hr
  3. filtrationThe hot reaction mixture was filtered
  4. customto remove an amorphous solid
  5. customThe product persistently crystallized in the filter
  6. customThe product was recrystallized from acetone
  7. customrecovered
  8. washwashing the residue with cold acetone
  9. customto give 27 g of large, off-white crystals, mp 178°-182° C.

출처 및 근거

ORD 기록
ord-fc9eb7368e2b469eb2cd728059584241
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04826866

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