Ammonium Chloride → HCID 23325186、化合物

HRID 1380487ノート

反応式

HRID 1380487 の反応式
[Na].C[Si](C)(C)[C:4]#[C:5][CH:6]([N:13]=[CH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:7][CH2:8][C:9]([O:11][CH3:12])=[O:10].[Cl-].[NH4+]>CO>[CH:14](=[N:13][CH:6]([C:5]#[CH:4])[CH2:7][CH2:8][C:9]([O:11][CH3:12])=[O:10])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 13780253Methyl 4-[(phenylmethylene)amino]-6-(trimethylsilyl)-5-hexynoate

生成物 1

HCID 23325186HCID 23325186、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

0.0764 g of sodium was dissolved in 5 ml of methanol. The solution was added at room temperature to a solution of 1.0 g of 3A in 2 ml of dry methanol. The mixture was stirred at room temperature for 4 hours, then 0.1765 g of ammonium chloride was added and the mixture was stirred for 15 minutes. Then the methanol was evaporated, the residue was triturated with ether and the solid phase was filtered off. The solvent was evaporated from the filtrate and the residue was distilled to give 4, b.p.: 170° C. (0.07 Torr).

後処理

  1. stirringthe mixture was stirred for 15 minutes
  2. customThen the methanol was evaporated
  3. customthe residue was triturated with ether
  4. filtrationthe solid phase was filtered off
  5. customThe solvent was evaporated from the filtrate
  6. distillationthe residue was distilled
  7. customto give 4, b.p.: 170° C. (0.07 Torr)

出典と根拠

ORDレコード
ord-694019a6c8ad45ccb28cbe5e11874e9f
出典データセット
uspto-grants-1986_04
特許番号
US04582529

反応ノート

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