Stannous chloride dihydrate → HCID 69145987、化合物

HRID 444963ノート

反応式

HRID 444963 の反応式
O.O.[Sn](Cl)Cl.[CH2:6]([N:9]1[CH2:14][CH2:13][N:12]([C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][N:16]=2)[CH2:11][CH:10]1[CH3:24])[CH:7]=[CH2:8]>CO>[CH2:6]([N:9]1[CH2:14][CH2:13][N:12]([C:15]2[N:16]=[CH:17][C:18]([NH2:21])=[CH:19][CH:20]=2)[CH2:11][CH:10]1[CH3:24])[CH:7]=[CH2:8]

参加物

4

反応物 2

HCID 61436Stannous chloride dihydrateHCID 691459762-Methyl-4-(5-nitro-2-pyridinyl)-1-(2-propen-1-yl)piperazine

生成物 1

HCID 69145987HCID 69145987、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

4.975 g (22.05 mmol) of tin(II) chloride dihydrate were added to a solution of 707 mg (2.45 mmol) of 1-allyl-2-methyl-4-(5-nitropyridin-2-yl)piperazine from Example 13.2 in 50 ml of methanol and the resulting mixture was stirred at 70° C. for 90 minutes. After the solvent had been evaporated down to dryness, water was added to the resulting residue and the mixture was made alkaline using a dilute aqueous solution of sodium hydroxide. After that, the aqueous reaction mixture was extracted with ethyl acetate. The solid which had precipitated out was filtered off with suction and the phases were separated. The aqueous phase was extracted with dichloromethane. After that, the combined organic phases were dried over sodium sulfate, filtered and evaporated down to dryness. The resulting title compound was used in the next step without any further purification.

後処理

  1. customAfter the solvent had been evaporated down to dryness, water
  2. additionwas added to the resulting residue
  3. extractionAfter that, the aqueous reaction mixture was extracted with ethyl acetate
  4. customThe solid which had precipitated out
  5. filtrationwas filtered off with suction
  6. customthe phases were separated
  7. extractionThe aqueous phase was extracted with dichloromethane
  8. dry with materialAfter that, the combined organic phases were dried over sodium sulfate
  9. filtrationfiltered
  10. customevaporated down to dryness
  11. customThe resulting title compound was used in the next step without any further purification

出典と根拠

ORDレコード
ord-b337d0cf5a9d4bc0b2f4bbdf87b01f49
出典データセット
uspto-grants-2013_07
特許番号
US08476275B2

反応ノート

読み込み中…