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

HRID 35434

反応式

HRID 35434 の反応式
[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]

参加物

8

反応物 5

HCID 111,2-DichloroethaneHCID 335O-Cresol2 回HCID 6397ChlorotrimethylsilaneHCID 7967CyclohexanoneHCID 8012Butanethiol

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8078Cyclohexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-67f58ef83fb54c28be9b4493e5d1da62
出典データセット
uspto-grants-1988_08
特許番号
US04766255

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