Allene → 1,2,4-Trimethylenecyclohexane

HRID 2399435

反応式

HRID 2399435 の反応式
[CH2:1]=[C:2]=[CH2:3].C=C1CCC1=C.[CH2:10]=[C:11]1[CH2:14][C:13](=[CH2:15])[CH2:12]1>>[CH2:1]=[C:2]1[CH2:3][CH2:12][C:13](=[CH2:15])[CH2:14][C:11]1=[CH2:10]

参加物

4

反応物 3

HCID 10037Allene2 回HCID 1372971,3-Bis(methylene)cyclobutaneHCID 139725Cyclobutane, 1,2-bis(methylene)-

生成物 1

HCID 5707051,2,4-Trimethylenecyclohexane

実験手順

The system was first purged with nitrogen. The power to the fluidized bed was turned on and its temperature was brought to 450°-470° C. Allene was introduced into the system from the allene cylinder at a rate of 80-100 grams/hour. The allene supply from the cylinder was shut off two to three hours before the end of a dimerization run in order that the allene present in the system could be used up, with little allene remaining in the reservoir a the end. At the end of the day, the power to the fluidized bed was turned off, the system was allowed to cool, and the accumulated crude liquid product was poured into a bottle and weighed. Approximately 3 grams of phenothiazine was added per kilogram of crude liquid product to inhibit polymerization and oxidation of the dimers and trimers. The crude product was then analyzed by gas chromatography for peaks corresponding to two allene dimers, 1,2-dimethylenecyclobutane (1,2-DMCB) and 1,3-dimethylenecyclobutane (1,3-DMCB), and the allene trimer 1,2,4-trimethylenecyclohexane (TMCH). Data from seven hot tube reaction runs are shown in Table 1.

後処理

  1. customThe system was first purged with nitrogen
  2. customwas brought to 450°-470° C
  3. additionAllene was introduced into the system from the allene cylinder at a rate of 80-100 grams/hour
  4. waitThe allene supply from the cylinder was shut off two to three hours before the end of a dimerization run in order that the allene present in the system
  5. temperatureto cool
  6. additionwas poured into a bottle
  7. additionApproximately 3 grams of phenothiazine was added per kilogram of crude liquid product
  8. custompolymerization and oxidation of the dimers and trimers
  9. customData from seven hot tube reaction runs

出典と根拠

ORDレコード
ord-0905a119ad0b4bf38bbcbc2fd58e504c
出典データセット
uspto-grants-1995_09
特許番号
US05449726

関連ノート

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