Acetic Anhydride → 5,5'-Carbonyldi(2-benzofuran-1,3-dione)--1-(4-aminophenyl)-1,3,3-trimethyl-2,3-dihydro-1H-inden-5-amine (1/1)

HRID 2067301

反応式

HRID 2067301 の反応式
N[CH2:2][CH2:3]CCCCCCCCCCN.N[CH2:16]CC[Si](C)(C)O[Si](C)(C)[CH2:22][CH2:23][CH2:24][NH2:25].C[C:31]([C:51]1[CH:56]=CC(OC2C=CC3C(OC(=O)C=3C=2)=O)=C[CH:52]=1)([C:33]1[CH:38]=C[C:36](O[C:40]2[CH:45]=[CH:44][C:43]3[C:46]([O:48][C:49](=[O:50])[C:42]=3[CH:41]=2)=[O:47])=[CH:35][CH:34]=1)C.[C:69]([O:72][C:73](=[O:75])[CH3:74])(=[O:71])[CH3:70].C[N:77]1[CH2:81][CH2:80][CH2:79][C:78]1=[O:82]>O>[CH3:52][C:51]1([CH3:56])[C:79]2[CH:80]=[C:81]([NH2:77])[CH:2]=[CH:3][C:78]=2[C:33]([C:34]2[CH:22]=[CH:23][C:24]([NH2:25])=[CH:36][CH:35]=2)([CH3:38])[CH2:31]1.[CH:45]1[C:40]([C:78]([C:79]2[CH:80]=[CH:81][C:70]3[C:69]([O:72][C:73](=[O:75])[C:74]=3[CH:16]=2)=[O:71])=[O:82])=[CH:41][C:42]2[C:49]([O:48][C:46](=[O:47])[C:43]=2[CH:44]=1)=[O:50]

参加物

7

反応物 5

HCID 7918Acetic AnhydrideHCID 13387N-methyl-2-pyrrolidoneHCID 171813,3'-(1,1,3,3-Tetramethyldisiloxane-1,3-diyl)bispropylamineHCID 177271,12-DodecanediamineHCID 944832,2-Bis(4-(3,4-dicarboxyphenoxy)phenyl)propane dianhydride

生成物 1

HCID 64544855,5'-Carbonyldi(2-benzofuran-1,3-dione)--1-(4-aminophenyl)-1,3,3-trimethyl-2,3-dihydro-1H-inden-5-amine (1/1)

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
180 °C

実験手順

A 300 ml flask fitted with a thermometer, a stirrer, a condenser, and a nitrogen inlet tube was charged with 2.71 g (0.045 mols) of 1,12-diaminododecane, 5.77 g (0.01 mols) of a polyetherdiamine (ED2000 (a product name), manufactured by BASF Corporation, molecular weight: 1,923), 3.35 g (0.045 mols) of 1,3-bis(3-aminopropyl)tetramethyldisiloxane (LP-7100 (a product name), manufactured by Shin-Etsu Chemical Co., Ltd.), 15.62 g (0.1 mols) of 4,4′-(4,4′-isopropylidenediphenoxy)bis(phthalic anhydride) that had been purified in advance by recrystallization from acetic anhydride (and exhibited a difference between the endothermic start temperature and the endothermic peak temperature as determined by DSC of 2.5° C.), and 113 g of N-methyl-2-pyrrolidone, and the resulting reaction liquid was then heated to 180° C. under constant stirring while nitrogen gas was blown through the system, thereby allowing the reaction to progress. The water generated within the reaction liquid was then removed, yielding a solution of a polyimide resin (PI-C). Measurement of the polyimide resin by GPC revealed polystyrene equivalent values of Mn=22,600 and Mw=121,400.

後処理

  1. customA 300 ml flask fitted with a thermometer, a stirrer, a condenser, and a nitrogen inlet tube
  2. customas determined by DSC of 2.5° C.
  3. customthe resulting reaction liquid
  4. customthe reaction
  5. customwas then removed

出典と根拠

ORDレコード
ord-036188e68d7d42a5bc37ef0dee03a5db
出典データセット
uspto-grants-2012_10
特許番号
US08293847B2

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