Hydrochloric Acid → HCID 20326723, 화합물

HRID 372826노트

반응식

HRID 372826 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 20326723HCID 20326723, 화합물

시약·촉매·용매 1

HCID 241Benzene용매2회

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-106176af991a49b79f78e9606ad45480
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04092344

반응 노트

불러오는 중…