Sodium Iodide → HCID 14456867、化合物

HRID 279781ノート

反応式

HRID 279781 の反応式
[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH:9]([CH2:10]OS(C)(=O)=O)[CH2:8][C:7]1=[O:16].[I-:23].[Na+]>CC(C)=O>[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH:9]([CH2:10][I:23])[CH2:8][C:7]1=[O:16]

参加物

4

反応物 2

HCID 5238Sodium Iodide2 回HCID 13505934HCID 13505934、化合物

生成物 1

HCID 14456867HCID 14456867、化合物収率 104.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 37.5 g (0.107 mole) of 1-(2,4-dimethoxy-benzyl)-4-(mesyloxymethyl)-2-azetidinone prepared according to the preceding paragraph, 250 ml of anhydrous acetone, and 56.3 g (0.376 mole) of sodium iodide is heated to boiling for 8 hours. To the mixture a further amount of 18.8 g (0.125 mole) of sodium iodide are added and the mixture is stirred for a further 8 hours under boiling. The mixture is evaporated to dryness on a water-bath (internal temperature 50° C.), the residue is rubbed with 100 ml of water and the oil thus obtained is extracted with 100 ml of dichloromethane. The aqueous layer is extracted three times with 50 ml of dichloromethane each. The united dichloromethane layers are dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated. Thus 40.3 g of 1-(2,4-dimethoxy-benzyl)-4-(iodomethyl)-2-azetidinone are obtained. Yield: 98%.

後処理

  1. customprepared
  2. temperatureis heated
  3. customThe mixture is evaporated to dryness on a water-bath (internal temperature 50° C.)
  4. customthe oil thus obtained
  5. extractionis extracted with 100 ml of dichloromethane
  6. extractionThe aqueous layer is extracted three times with 50 ml of dichloromethane each
  7. dry with materialThe united dichloromethane layers are dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customthe filtrate is evaporated

出典と根拠

ORDレコード
ord-b4e36deae4a942f78db7fcfcdd295c3f
出典データセット
uspto-grants-1986_05
特許番号
US04587049

反応ノート

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