Hydrochloric Acid → HCID 20326723、化合物

HRID 372826ノート

反応式

HRID 372826 の反応式
[H-].COCCO[Al+]OCCOC.[Na+].[H-].[OH:15][C:16]1[C:25]2[C:24]3[CH2:26][CH:27]([CH3:30])[CH2:28][CH2:29][C:23]=3[C:22](=[O:31])[O:21][C:20]=2[CH:19]=[C:18]([CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[CH:17]=1.Cl>C1C=CC=CC=1>[OH:31][CH2:22][C:23]1[CH2:29][CH2:28][CH:27]([CH3:30])[CH2:26][C:24]=1[C:25]1[C:16]([OH:15])=[CH:17][C:18]([CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])=[CH:19][C:20]=1[OH:21]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 53584061-hydroxy-9-methyl-3-pentyl-7,8,9,10-tetrahydrobenzo[c]chromen-6-oneHCID 21584525Sodium bis(2-methoxyethoxy)aluminiumhydride

生成物 1

HCID 20326723HCID 20326723、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

反応条件

温度
25 °C

実験手順

A solution of 90 ml. of a seventy percent solution of sodium bis(2-methoxyethoxy)aluminum hydride in 80 ml. of benzene was cooled in an ice-water bath and stirred while a suspension of 13.0 g. of 1-hydroxy-3-n-pentyl-6-oxo-9-methyl-7,8,9,10-tetrahydro-6H-dibenzo[b,d]pyran in 220 ml. of benzene was added portion-wise over 15 minutes. The reaction mixture was warmed to about 25° C. and stirred for 2 hours. The reaction mixture was again cooled in an ice-water bath and stirred while 800 ml. of 10 percent aqueous hydrochloric acid solution was added. The aqueous acidic reaction mixture was extracted several times with diethyl ether. The ethereal extracts were combined, washed with water, and dried. Removal of the solvent under reduced pressure provided 2-(2-hydroxymethyl-5-methyl-1-cyclohexenyl)-5-n-pentyl-resorcinol as a white crystalline solid. M.P. 109°-11° C.

後処理

  1. stirringstirred for 2 hours
  2. temperatureThe reaction mixture was again cooled in an ice-water bath
  3. stirringstirred while 800 ml
  4. extractionThe aqueous acidic reaction mixture was extracted several times with diethyl ether
  5. washwashed with water
  6. customdried
  7. customRemoval of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-106176af991a49b79f78e9606ad45480
出典データセット
uspto-grants-1978_05
特許番号
US04092344

反応ノート

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