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Water → Sodium 3,5-di-(2,4-di-tert-amylphenoxypropylcarbamoyl)benzenesulfinate

HRID 4877
ノート
印刷プレビュー

反応式

HRID 4877 の反応式
S([O-])([O-])=O.[Na+:5].[Na+].C(=O)([O-])O.[Na+].O.[C:13]([CH:18]([CH2:56][O:57][C:58]1[CH:63]=[CH:62][C:61]([C:64]([CH2:67][CH3:68])([CH3:66])[CH3:65])=[CH:60][CH:59]=1)[CH2:19][NH:20][C:21]([C:23]1[CH:24]=[C:25]([S:52](Cl)(=[O:54])=[O:53])[CH:26]=[C:27]([C:29](=[O:51])[NH:30][CH2:31][CH:32]([C:46]([CH2:49][CH3:50])([CH3:48])[CH3:47])[CH2:33][O:34][C:35]2[CH:40]=[CH:39][C:38]([C:41]([CH2:44][CH3:45])([CH3:43])[CH3:42])=[CH:37][CH:36]=2)[CH:28]=1)=[O:22])([CH2:16][CH3:17])([CH3:15])[CH3:14]>C(#N)C>[C:13]([CH:18]([CH2:56][O:57][C:58]1[CH:59]=[CH:60][C:61]([C:64]([CH2:67][CH3:68])([CH3:65])[CH3:66])=[CH:62][CH:63]=1)[CH2:19][NH:20][C:21]([C:23]1[CH:24]=[C:25]([S:52]([O-:54])=[O:53])[CH:26]=[C:27]([C:29](=[O:51])[NH:30][CH2:31][CH:32]([C:46]([CH2:49][CH3:50])([CH3:47])[CH3:48])[CH2:33][O:34][C:35]2[CH:40]=[CH:39][C:38]([C:41]([CH2:44][CH3:45])([CH3:43])[CH3:42])=[CH:37][CH:36]=2)[CH:28]=1)=[O:22])([CH2:16][CH3:17])([CH3:14])[CH3:15].[Na+:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24437Sodium SulfiteHCID 516892Sodium BicarbonateHCID 867440573,5-Di-(2,4-di-tert-amylphenoxypropylcarbamoyl)benzenesulfonyl chloride

生成物 1

HCID 67635903Sodium 3,5-di-(2,4-di-tert-amylphenoxypropylcarbamoyl)benzenesulfinate収率 82.8%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒
2 回

反応条件

温度
30 °C

実験手順

To 2 g (0.016 mol) of sodium sulfite and 2.4 g (0.029 mol) of sodium hydrogen carbonate were added 100 ml of water and 20 ml of acetonitrile and the mixture was stirred at 30° C. To the mixture was added dropwise a solution of 10.5 g (0.013 mol) of 3,5-di-(2,4-di-tert-amylphenoxypropylcarbamoyl)benzenesulfonyl chloride obtained in the aforesaid step dissolved in 100 ml of acetonitrile. After stirring the resultant mixture for one hour, the reaction mixture was poured onto ice water and extracted with 150 ml of ethyl acetate. The ethyl acetate layer was washed thrice with cold water and dried over Glauber's salt. After filtrating away the Glauber's salt, the residue was concentrated to dryness to provide 8.6 g (yield of 82.8%) of a solid product.

後処理

  1. customobtained in the aforesaid step
  2. additionthe reaction mixture was poured onto ice water
  3. extractionextracted with 150 ml of ethyl acetate
  4. washThe ethyl acetate layer was washed thrice with cold water
  5. dry with materialdried over Glauber's salt
  6. filtrationAfter filtrating away the Glauber's salt
  7. concentrationthe residue was concentrated to dryness

出典と根拠

ORDレコード
ord-1552f7df163c4dd28c6db945c2a62da2
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05242785

反応ノート

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