Hydrochloric Acid → HCID 20149481、化合物

HRID 568974ノート

反応式

HRID 568974 の反応式
[NH2:1][C:2]([C:16]([O:18]CC)=[O:17])([CH2:8][CH2:9][CH:10]([F:15])[CH:11]([NH2:14])[CH:12]=[CH2:13])[C:3]([O:5]CC)=[O:4].[OH-].[Na+].Cl.C1OC1C>C(O)C.C(O)(C)C>[NH2:1][C:2]([C:16]([OH:18])=[O:17])([CH2:8][CH2:9][CH:10]([F:15])[CH:11]([NH2:14])[CH:12]=[CH2:13])[C:3]([OH:5])=[O:4]

参加物

7

反応物 4

HCID 313Hydrochloric Acid2 回HCID 6378Propylene OxideHCID 14798Sodium HydroxideHCID 20149487HCID 20149487、化合物

生成物 1

HCID 20149481HCID 20149481、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3776Isopropanol溶媒

実験手順

The crude material 23 (11.5 g, about 31 mmoles since some solvent left) is dissolved in ethanol (150 mL) and 2N NaOH (150 mL) and stirred at room temperature for 3 hours. The mixture is neutralized with conc. HCl (about 25 mL) with cooling, then acidified (HCl). After evaporation and drying, the residue is dissolved in ethanol, filtered through millipore, and evaporated again. Dissolving in water, filtration, and evaporation yields a solid (11 g, 2 g more than theory). This is dissolved in isopropanol (130 mL) and treated with propylene oxide (6.5 mL, 3 equivalents). Crude 24 (7.2 g, somewhat more than theory) is collected. Thin layer chromatography (ethanol/NH4OH 80/20 revelation ninhydrin) indicates the presence of some decarboxylated product. The compound 24 is used without further purification. Recrystallization from water/ethanol is possible. Caution: no heating!

後処理

  1. temperaturewith cooling
  2. customAfter evaporation
  3. customdrying
  4. dissolutionthe residue is dissolved in ethanol
  5. filtrationfiltered through millipore
  6. customevaporated again
  7. dissolutionDissolving in water
  8. filtrationfiltration, and evaporation
  9. customyields a solid (11 g, 2 g more than theory)
  10. customCrude 24 (7.2 g, somewhat more than theory) is collected
  11. customThe compound 24 is used without further purification
  12. customRecrystallization from water/ethanol

出典と根拠

ORDレコード
ord-409d3eeb86f647a9beb79440f12b5c41
出典データセット
uspto-grants-1988_03
特許番号
US04730006

反応ノート

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