Allyl bromide → HCID 12884358、化合物

HRID 2199066ノート

反応式

HRID 2199066 の反応式
[CH3:1][N:2]1[CH2:6][CH2:5][NH:4][C:3]1=[N:7][C:8]1[C:13]([Cl:14])=[CH:12][CH:11]=[CH:10][C:9]=1[Cl:15].[CH2:16](Br)[CH:17]=[CH2:18].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH3:1][N:2]1[CH2:6][CH2:5][N:4]=[C:3]1[N:7]([CH2:18][CH:17]=[CH2:16])[C:8]1[C:9]([Cl:15])=[CH:10][CH:11]=[CH:12][C:13]=1[Cl:14]

参加物

5

反応物 3

HCID 7841Allyl bromideHCID 10340Sodium CarbonateHCID 178480594HCID 178480594、化合物

生成物 1

HCID 12884358HCID 12884358、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture consisting of 4.9 gm (0.02 mol) of 1-methyl-2-(2,6-dichlorophenyl-imino)-imidazolidine, 2.1 ml of allyl bromide (125% of the stoichiometrically required amount), 2.7 gm of sodium carbonate and 25 ml of ethanol was refluxed for 5.5 hours while stirring. Thereafter, the reaction mixture was filtered, the filtrate was evaporated in vacuo to dryness, the residue was dissolved in dilute (about 1 N) hydrochloric acid, and the resulting solution was extracted with ether (the ethanol extracts were discarded). The acidic aqueous phase was then fractionally extracted with ether at stepwisely increasing pH-values (addition of 2 N sodium hydroxide). The thin-layer chromatographically uniform fractions were combined, dried over magnesium sulfate, and the ether was evaporated in vacuo, leaving an oil which crystallized gradually throughout. 2.3 gm (40.5% of theory) of the compound of the formula ##STR7## having a melting point of 59°-61° C. were obtained.

後処理

  1. temperaturewas refluxed for 5.5 hours
  2. filtrationThereafter, the reaction mixture was filtered
  3. customthe filtrate was evaporated in vacuo to dryness
  4. dissolutionthe residue was dissolved
  5. additionin dilute (about 1 N) hydrochloric acid
  6. extractionthe resulting solution was extracted with ether (the ethanol extracts
  7. extractionThe acidic aqueous phase was then fractionally extracted with ether at stepwisely increasing pH-values (addition of 2 N sodium hydroxide)
  8. dry with materialdried over magnesium sulfate
  9. customthe ether was evaporated in vacuo
  10. customleaving an oil which
  11. customcrystallized gradually throughout
  12. customwere obtained

出典と根拠

ORDレコード
ord-9d1eafd63bba471ab317a7d4f42b2bf8
出典データセット
uspto-grants-1982_11
特許番号
US04361575

反応ノート

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