HCID 13731468, 화합물 → HCID 13731469, 화합물

HRID 2291027노트

반응식

HRID 2291027 반응식
[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.[CH2:12]([O:19][CH2:20][C:21]1([CH2:27][CH2:28][O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH3:47])[O:25][CH:24]([OH:26])[CH2:23][CH2:22]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(Cl)Cl.CCOCC>[CH2:12]([O:19][CH2:20][C:21]1([CH2:27][CH2:28][O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH3:47])[O:25][C:24](=[O:26])[CH2:23][CH2:22]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

5

반응물 2

HCID 13731468HCID 13731468, 화합물HCID 178418287HCID 178418287, 화합물

생성물 1

HCID 13731469HCID 13731469, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 1.6 g (7.4 mmol) of pyridinium chlorochromate in 25 ml of methylene chloride under a nitrogen atmosphere, was added 13.5 g (6.5 mmol) of the compound prepared in (d) above in 25 ml of methylene chloride. After 18 hours at 25° C., the solution was diluted with 150 ml of ether, filtered through silica gel and the filtrate evaporated to afford an oil. The oil was then flash chromatographed on silica gel employing a mixture of petroleum ether and diethyl ether in a ratio of 7:3 as the eluent to yield colorless oil.

후처리

  1. filtrationfiltered through silica gel
  2. customthe filtrate evaporated
  3. customto afford an oil
  4. customflash chromatographed on silica gel employing
  5. additiona mixture of petroleum ether and diethyl ether in a ratio of 7:3 as the eluent
  6. customto yield colorless oil

출처 및 근거

ORD 기록
ord-09eaaa1f2dfa431ebcf2139a7972f4cf
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04619917

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