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Hydrochloric Acid → HCID 67916362, 화합물

HRID 1534298
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HRID 1534298 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 23667635Sodium periodateHCID 67916399HCID 67916399, 화합물

생성물 1

HCID 67916362HCID 67916362, 화합물수율 21.2%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매2회
HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8b936192a60b4a35af13b65b09eb33d7
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05087743

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