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Hydrochloric Acid → HCID 67916362、化合物

HRID 1534298
ノート
印刷プレビュー

反応式

HRID 1534298 の反応式
I([O-])(=O)(=O)=[O:2].[Na+].[C:7]([C:10]1[CH:55]=[CH:54][C:13]([CH2:14][C:15]2[C:24]3[C:23]([CH3:26])([CH3:25])[CH2:22][CH2:21][C:20]([CH3:28])([CH3:27])[C:19]=3[CH:18]=[CH:17][C:16]=2[S:29][C:30]2[CH:39]=[CH:38][C:37]3[C:36]([CH3:41])([CH3:40])[CH2:35][CH2:34][C:33]([CH3:43])([CH3:42])[C:32]=3[C:31]=2[CH2:44][C:45]2[CH:50]=[CH:49][C:48]([C:51]([OH:53])=[O:52])=[CH:47][CH:46]=2)=[CH:12][CH:11]=1)([OH:9])=[O:8].Cl>O.C(O)C.CN(C)C=O>[C:7]([C:10]1[CH:11]=[CH:12][C:13]([CH2:14][C:15]2[C:24]3[C:23]([CH3:25])([CH3:26])[CH2:22][CH2:21][C:20]([CH3:27])([CH3:28])[C:19]=3[CH:18]=[CH:17][C:16]=2[S:29]([C:30]2[CH:39]=[CH:38][C:37]3[C:36]([CH3:41])([CH3:40])[CH2:35][CH2:34][C:33]([CH3:42])([CH3:43])[C:32]=3[C:31]=2[CH2:44][C:45]2[CH:50]=[CH:49][C:48]([C:51]([OH:53])=[O:52])=[CH:47][CH:46]=2)=[O:2])=[CH:54][CH:55]=1)([OH:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 23667635Sodium periodateHCID 67916399HCID 67916399、化合物

生成物 1

HCID 67916362HCID 67916362、化合物収率 21.2%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒2 回
HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3.4 g (16 mmol) of sodium periodate in 30 ml of water was added dropwise to 5.3 g (15 mmol) of the thioether from Example 10 in a mixture of 150 ml of ethanol and 40 ml of dimethylformamide at 0° C., and the mixture was then stirred at the same temperature for 2 hours and at room temperature overnight. The reaction solution was then poured into water, the pH was adjusted to 5 with 2N hydrochloric acid, the mixture was extracted with dichloromethane, and the organic extracts were washed with water, dried over magnesium sulfate and evaporated under reduced pressure. Crystallization of the oily residue from ethanol yielded 2.2 g of title compound of melting point 198°-200° C.

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. washthe organic extracts were washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure
  5. customCrystallization of the oily residue from ethanol

出典と根拠

ORDレコード
ord-8b936192a60b4a35af13b65b09eb33d7
出典データセット
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05087743

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート