Benzene → HCID 20364884, 화합물

HRID 1678998노트

반응식

HRID 1678998 반응식
[H-].[Na+].C1C=CC=CC=1.[OH:9][CH:10]1[CH2:15][O:14][CH:13]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[CH:17]=2)[O:12][CH2:11]1.[CH2:23](Cl)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C1(C)C(C)=CC=CC=1>[CH2:23]([O:9][CH:10]1[CH2:11][O:12][CH:13]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[CH:17]=2)[O:14][CH2:15]1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

6

반응물 4

HCID 241BenzeneHCID 7503Benzyl ChlorideHCID 24758Sodium hydrideHCID 203649382-(3-Methylphenyl)-1,3-dioxan-5-ol

생성물 1

HCID 20364884HCID 20364884, 화합물수율 91.9%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A slurry of sodium hydride (2.1 g. 0.08 mole in 100 ml of xylene and 100 ml of benzene was stirred at ambient temperature while 5-hydroxy-2-(3-methylphenyl)-1,3-dioxane (15.9 g, 0.08 mole) was added dropwise during 1 hour. Stirring was continued for one hour and to the mixture was added benzyl chloride (10.4 g, 0.08 mole) during 0.5 hour. This mixture was heated under reflux for 22 hours, cooled, filtered and the filtrate washed with water (2 × 250 ml). The washed solution was dried over magnesium sulfate and concentrated under reduced pressure to give 20.9 g of oil which distilled at 2 × 10-4 mm. to give three fractions distilling respectively at 102°-133° C (cut 1); 133°-141° C (cut 2); and 141° C (cut 3). Analysis of the various cuts indicated that cut 3 was essentially pure cis-5 -benzyloxy-2-(3-methylphenyl)-1,3-dioxane, 2.1 g, m.p. 68°-70° C and this cut was used in further studies.

후처리

  1. additionwas added dropwise during 1 hour
  2. temperatureThis mixture was heated
  3. temperatureunder reflux for 22 hours
  4. temperaturecooled
  5. filtrationfiltered
  6. washthe filtrate washed with water (2 × 250 ml)
  7. dry with materialThe washed solution was dried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d6cb5460598b44559658d2b8eab82672
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04077982

반응 노트

불러오는 중…