Sodium Iodide → HCID 131729476、化合物

HRID 1645411ノート

反応式

HRID 1645411 の反応式
[CH2:1]1[S:9](=[O:11])(=[O:10])[O:8][CH2:7][CH2:6][O:5][S:2]1(=[O:4])=[O:3].[H-].[Na+].Cl[CH2:15][C:16]1[C:25]2[C:20](=CC=C[CH:24]=2)[CH:19]=[CH:18][CH:17]=1.[Na+].[I-].[CH2:28]([CH2:31]OC)OC>>[CH:24]1[C:25]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:6][C:7]=1[O:8][S:9]([CH:1]([S:2]([OH:5])(=[O:4])=[O:3])[CH3:28])(=[O:11])=[O:10].[CH2:28]=[CH2:31]

参加物

6

反応物 5

HCID 5238Sodium IodideHCID 68451-ChloromethylnaphthaleneHCID 80711,2-DimethoxyethaneHCID 24758Sodium hydrideHCID 57513Cyclodisone

生成物 1

HCID 131729476HCID 131729476、化合物収率 86%

実験手順

To a solution of 3.5 g of ethylene methanedisulfonate in 60 mL of glyme and 0.9 g of NaH was added 3.4 g of 1-chloromethylnaphthalene followed by 2.6 g of NaI. The solution was stirred overnight and the glyme removed by the rotary evaporator at 20 mm pressure. The residue was taken up in an acid solution and CH2Cl2. The CH2Cl2 was rinsed with a NaHSO3 solution, dried, concentrated, and cyclohexane was added to give 3.9 g (86%) of ethylene 2-naphthyl-1,1-ethanedisulfonate, m.p. 179-183° C. (94-2).

後処理

  1. customthe glyme removed by the rotary evaporator at 20 mm pressure
  2. washThe CH2Cl2 was rinsed with a NaHSO3 solution
  3. customdried
  4. concentrationconcentrated
  5. additioncyclohexane was added

出典と根拠

ORDレコード
ord-345c017f3a8b405a8e8100fe5c8afcba
出典データセット
uspto-grants-2012_02
特許番号
US08124793B2

反応ノート

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