1,2-Dichloroethane → Phenol, 4,4'-cyclohexylidenebis[2-methyl-

HRID 35434

반응식

HRID 35434 반응식
[C:1]1([CH3:8])[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:9]1(=[O:15])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.Cl[Si](C)(C)[CH3:18].[CH2:21](S)[CH2:22][CH2:23][CH3:24].Cl[CH2:27][CH2:28]Cl>C(Cl)Cl.C1CCCCC1>[CH3:8][C:1]1[CH:2]=[C:3]([C:21]2([C:12]3[CH:13]=[CH:14][C:9]([OH:15])=[C:10]([CH3:18])[CH:11]=3)[CH2:28][CH2:27][CH2:24][CH2:23][CH2:22]2)[CH:4]=[CH:5][C:6]=1[OH:7]

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 335O-Cresol2회HCID 6397ChlorotrimethylsilaneHCID 7967CyclohexanoneHCID 8012Butanethiol

생성물 1

HCID 75386Phenol, 4,4'-cyclohexylidenebis[2-methyl-수율 76%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8078Cyclohexane용매

실험 절차

The preparation of the above cyclohexane was accomplished by repeating the procedure of Example I with the exception that o-cresol was employed in place of phenol. In addition, the preparation was affected in a 250-milliliter 3-necked round-bottomed flask with 0.2 mole of cyclohexanone, and without 1,2-dichloroethane as a solvent. Additionally, 108 grams of o-cresol, 22 grams of chlorotrimethyl silane, and 0.1 gram of butanethiol were employed. The reaction mixture was worked up by filtering it hot after the reaction, followed by slurrying up the filter cake in methylene chloride, filtering and washing several times with methylene chloride. There was obtained the cyclohexane product in a 76 percent yield after drying in vacuo at 80° C. for 12 hours, which product had a melting point of 190° to 191° C.

후처리

  1. filtrationby filtering it
  2. customhot after the reaction
  3. filtrationfiltering
  4. washwashing several times with methylene chloride
  5. customThere was obtained the cyclohexane product in a 76 percent yield
  6. customafter drying in vacuo at 80° C. for 12 hours

출처 및 근거

ORD 기록
ord-67f58ef83fb54c28be9b4493e5d1da62
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766255

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