HCID 13731468、化合物 → HCID 13731469、化合物

HRID 2291027ノート

反応式

HRID 2291027 の反応式
[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

参加物

5

反応物 2

HCID 13731468HCID 13731468、化合物HCID 178418287HCID 178418287、化合物

生成物 1

HCID 13731469HCID 13731469、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09eaaa1f2dfa431ebcf2139a7972f4cf
出典データセット
uspto-grants-1986_10
特許番号
US04619917

反応ノート

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