1,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate) → p-Hydroxystyrene p-tert-butoxystyrene

HRID 970262

反応式

HRID 970262 の反応式
C([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH2:10])=[CH:7][CH:6]=1)(=O)C.[C:13]([O:17][C:18]1[CH:25]=[CH:24][C:21]([CH:22]=[CH2:23])=[CH:20][CH:19]=1)([CH3:16])([CH3:15])[CH3:14].N(C(C)(CC)C([O-])=O)=NC(C)(CC)C([O-])=O.N(C(C)(C)C(OC)=O)=NC(C)(C)C(OC)=O>C(O)(C)C.O>[OH:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH2:10])=[CH:7][CH:6]=1.[C:13]([O:17][C:18]1[CH:19]=[CH:20][C:21]([CH:22]=[CH2:23])=[CH:24][CH:25]=1)([CH3:16])([CH3:14])[CH3:15]

参加物

7

反応物 4

HCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)HCID 758214-Ethenylphenyl acetateHCID 5775311-(Tert-butoxy)-4-ethenylbenzeneHCID 219175032,2'-Azobis(methyl 2-methylpropanate)

生成物 1

HCID 68598693p-Hydroxystyrene p-tert-butoxystyrene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3776Isopropanol溶媒

実験手順

In 400 mL of isopropanol, 56.7 g of p-acetoxystyrene and 26.4 g of p-tert-butoxystyrene were dissolved, then 8.3 g of 2,2′-azobis(methyl 2-methylpropionate) (V-601: trade name of a product from Wako Pure Chemicals Ind., Ltd.) was added, followed by reacting at 80° C. for 6 hours under nitrogen gas flow. After the reaction, said reaction solution obtained was poured into 10 L of water for precipitation, followed by filtering off deposited crystal. The thus obtained crystal was added to 450 mL of methanol, followed by charging 234 g of a 15% aqueous tetramethylammonium hydroxide solution and reacting under reflux for 4 hours while stirring. The thus obtained solution was cooled to room temperature, then neutralized by adding drop-wise 12.9 g of glacial acetic acid. The neutral solution was poured into 10 L of water for precipitation, followed by filtering off deposited crystal and drying under reduced pressure, to obtain 42.6 g of poly(p-hydroxystyrene/p-tert-butoxystyrene) as a white powder crystal. The thus obtained crystal was named polymer A1. A composition ratio of p-hydroxystyrene unit and p-tert-butoxystyrene unit in polymer A1 was found to be about 7:3 from the measurement results by 13CNMR. Weight average molecular weight (Mw) of polymer A1 was about 9,500 and distribution (Mw/Mn) thereof was about 1.75 from the measurement results by gel permeation chromatography using polystyrene as a standard.

後処理

  1. addition) was added
  2. customAfter the reaction
  3. customreaction solution
  4. customobtained
  5. filtrationby filtering off
  6. additionThe thus obtained crystal was added to 450 mL of methanol
  7. temperatureunder reflux for 4 hours
  8. additionby adding drop-wise 12.9 g of glacial acetic acid
  9. additionThe neutral solution was poured into 10 L of water for precipitation
  10. filtrationby filtering off
  11. customdrying under reduced pressure

出典と根拠

ORDレコード
ord-9f0dd3f7eabe4946877c9b757baa9675
出典データセット
uspto-grants-2007_12
特許番号
US07312014B2

関連ノート

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