Phenol → HCID 67079797、化合物

HRID 222845

反応式

HRID 222845 の反応式
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:8][CH:9]=[CH2:10].[CH3:11][CH:12]=[CH2:13].[CH3:14][CH:15]=[CH2:16].[CH3:17][CH:18]=[CH2:19].[CH3:20][CH:21]=[CH2:22].[H-].[Ca+2:24].[H-].[Ca]>>[Ca:24].[CH2:10]([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[OH:7])[CH2:9][CH2:8][CH2:13][CH2:12][CH2:11][CH2:16][CH2:15][CH2:14][CH2:19][CH2:18][CH2:17][CH2:20][CH2:21][CH3:22]

参加物

5

反応物 4

HCID 996PhenolHCID 2037991-Propene, pentamerHCID 3033859Calcium hydrideHCID 5460341Calcium

生成物 1

HCID 67079797HCID 67079797、化合物

反応条件

温度
13 °C

実験手順

Branched pentadecylphenol calcium salt was prepared from the alkylation of phenol with a branched chain C14-C18 olefin derived primarily from propylene pentamer. To a 2-liter round bottom flask equipped with a mechanical stirred, Dean Stark trap fitted with a condenser under an atmosphere of dry nitrogen was charged with 705 gm (2.32 moles) of a C15 branched alkylphenol followed by 500 gm of Chevron RLOP 100N oil. This mixture was cooled to approximately 13° C. using an ice bath and then 48.8 gm (1.16 moles) of calcium hydride (98% obtained from Aldrich Chemical Company) was added in approximately 10 gram portions with stirring. The reaction was then heated to 100° C. over 50 minutes and then heated to 200° C. for over 140 minutes and held at 200° C. for approximately 18 hours and then heated to 280° C. over 1 hour and held at 280° C. for 8.5 hours and then cooled to 230° C. and held at 230° C. for approximately 14 hours. The reaction was then cooled to 150° C. and filtered through a dry, hot (150° C.) 600 mL Buchner funnel containing a filter bed of Celite and maintained between 110° C. and 120° C. with the aid of a vacuum to afford a product containing 3.51 wt % calcium.

後処理

  1. customTo a 2-liter round bottom flask equipped with a mechanical stirred, Dean Stark trap
  2. customfitted with a condenser under an atmosphere of dry nitrogen
  3. temperatureThe reaction was then heated to 100° C. over 50 minutes
  4. temperatureheated to 200° C. for over 140 minutes
  5. temperatureheated to 280° C. over 1 hour
  6. waitheld at 280° C. for 8.5 hours
  7. temperaturecooled to 230° C.
  8. waitheld at 230° C. for approximately 14 hours
  9. temperatureThe reaction was then cooled to 150° C.
  10. filtrationfiltered through a dry, hot (150° C.) 600 mL Buchner funnel
  11. additioncontaining a filter bed of Celite
  12. temperaturemaintained between 110° C. and 120° C. with the aid of a vacuum
  13. customto afford a product

出典と根拠

ORDレコード
ord-89026591fcf6482bb6c6673d3fa3fb22
出典データセット
uspto-grants-2012_06
特許番号
US08207380B2

関連ノート

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