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Methanol → HCID 10997333, 화합물

HRID 2395242
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HRID 2395242 반응식
[CH:1]1(N=C=NC2CCCCC2)CCCCC1.[O:16]=[C:17]1[S:21][CH2:20][CH:19]([C:22]([OH:24])=[O:23])[CH2:18]1.CO>C(OCC)C.CN(C1C=CC=CN=1)C>[CH3:1][O:23][C:22]([CH:19]1[CH2:18][C:17](=[O:16])[S:21][CH2:20]1)=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 887MethanolHCID 10868DicyclohexylcarbodiimideHCID 31539575-oxothiolane-3-carboxylic acid

생성물 1

HCID 10997333HCID 10997333, 화합물수율 85.3%

시약·촉매·용매 2

HCID 218852-Dimethylaminopyridine촉매HCID 3283Diethyl Ether용매
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실험 절차

225 g (1.09 mol) of dicyclohexylcarbodiimide (DCC) are added in portions, while cooling with ice, to a solution of 160 g (1.095 mol) of tetrahydro-5-oxo-3-thiophenecarboxylic acid, 70 g (2.19 mol) of methanol and 4 g (32.8 mmol) of dimethylaminopyridine (DMAP) in 2.5 litres of diethyl ether. After 4 hours' stirring at room temperature, the dicyclohexylurea is filtered off and the filtrate is extracted with 500 ml of 2N hydrochloric acid and 500 ml of saturated sodium hydrogen carbonate solution, is washed with water and is dried over sodium sulfate. There are obtained 149 g of solid product having a melting point of 33°-35° C.

후처리

  1. filtrationthe dicyclohexylurea is filtered off
  2. extractionthe filtrate is extracted with 500 ml of 2N hydrochloric acid and 500 ml of saturated sodium hydrogen carbonate solution
  3. washis washed with water
  4. dry with materialis dried over sodium sulfate

출처 및 근거

ORD 기록
ord-763a0ab795d6455bbae084653ef8ca5e
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05814629

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