Hydrochloric Acid → HCID 14500702、化合物

HRID 1761545ノート

反応式

HRID 1761545 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 14500702HCID 14500702、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-fc9eb7368e2b469eb2cd728059584241
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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