Tricyclohexylphosphine → 5-Butylnorbornene 5-norbornene-2-carboxylic acid butyl ester 5-norbornene-2-carboxylic acid methyl ester

HRID 1270663

反応式

HRID 1270663 の反応式
[CH2:1]([CH:5]1[CH2:10][CH:9]2[CH2:11][CH:6]1[CH:7]=[CH:8]2)[CH2:2][CH2:3][CH3:4].[CH2:12]([O:16][C:17]([CH:19]1[CH2:24][CH:23]2[CH2:25][CH:20]1[CH:21]=[CH:22]2)=[O:18])[CH2:13][CH2:14][CH3:15].[CH3:26][O:27][C:28]([CH:30]1[CH2:35][CH:34]2[CH2:36][CH:31]1[CH:32]=[CH:33]2)=[O:29].FC1C([B-](C2C(F)=C(F)C(F)=C(F)C=2F)(C2C(F)=C(F)C(F)=C(F)C=2F)C2C(F)=C(F)C(F)=C(F)C=2F)=C(F)C(F)=C(F)C=1F.C[NH+](C)C1C=CC=CC=1.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1>C([O-])(=O)C.C([O-])(=O)C.[Pd+2].C1(C)C=CC=CC=1>[CH2:1]([CH:5]1[CH2:10][CH:9]2[CH2:11][CH:6]1[CH:7]=[CH:8]2)[CH2:2][CH2:3][CH3:4].[CH2:12]([O:16][C:17]([CH:19]1[CH2:24][CH:23]2[CH2:25][CH:20]1[CH:21]=[CH:22]2)=[O:18])[CH2:13][CH2:14][CH3:15].[CH3:26][O:27][C:28]([CH:30]1[CH2:35][CH:34]2[CH2:36][CH:31]1[CH:32]=[CH:33]2)=[O:29]

参加物

8

反応物 5

HCID 75806TricyclohexylphosphineHCID 168020Bicyclo[2.2.1]hept-2-ene, 5-butyl-2 回HCID 250075Methyl bicyclo[2.2.1]hept-5-ene-2-carboxylate2 回HCID 10996402N,N-dimethylanilinium tetrakis(pentafluorophenyl)borateHCID 15608148Butyl bicyclo[2.2.1]hept-5-ene-2-carboxylate2 回

生成物 1

HCID 866000195-Butylnorbornene 5-norbornene-2-carboxylic acid butyl ester 5-norbornene-2-carboxylic acid methyl ester

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 1140Toluene溶媒2 回

反応条件

温度
90 °C

実験手順

5-Butylnorbornene (35.8 g), 5-norbornene-2-carboxylic acid butyl ester (31.1 g) and 5-norbornene-2-carboxylic acid methyl ester (60.9 g) were added to a reactor at room temperature. Toluene (95.8 g) was added to the reactor. Air inside the reactor was replaced by nitrogen and the reactor was heated to 90° C. Palladium diacetate (22.4 mg), dimethyl aniliniumtetrakis (pentafluorophenyl)borate (160.2 mg) and tricylcohexylphosphine (28 mg) dissolved in dichloromethyl were added to the reactor. Reaction was performed for 18 hours while stirring to obtain a tricopolymer solution comprising 30 mol % of 5-butylnorbornene, 20 mol % of 5-norbornene-2-carboxylic acid butyl ester and 50 mol % of 5-norbornene-2-carboxylic acid methyl ester monomers. 287 g of toluene was added to dilute the solution. The copolymer had a molecular weight (Mw) of 175,000. The proportion of Mw/Mn was 2.13.

後処理

  1. additionwere added to the reactor
  2. customReaction
  3. customto obtain a tricopolymer solution
  4. additionto dilute the solution

出典と根拠

ORDレコード
ord-87ea5941c15a42f28171da8ceea4405a
出典データセット
uspto-grants-2007_04
特許番号
US07202312B2

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