Phthalimide → Bis(p-aminocyclohexyl)methane phthalamide

HRID 2166920

反応式

HRID 2166920 の反応式
[NH2:1][CH:2]1[CH2:7][CH2:6][CH:5]([CH2:8][CH:9]2[CH2:14][CH2:13][CH:12]([NH2:15])[CH2:11][CH2:10]2)[CH2:4][CH2:3]1.[C:16]1(=[O:26])[NH:20][C:19](=[O:21])[C:18]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:17]12>O>[C:16]([NH2:20])(=[O:26])[C:17]1[C:18](=[CH:22][CH:23]=[CH:24][CH:25]=1)[C:19]([NH2:1])=[O:21].[NH2:1][CH:2]1[CH2:3][CH2:4][CH:5]([CH2:8][CH:9]2[CH2:14][CH2:13][CH:12]([NH2:15])[CH2:11][CH2:10]2)[CH2:6][CH2:7]1

参加物

4

反応物 2

HCID 6809Phthalimide2 回HCID 156604,4'-Diaminodicyclohexylmethane

生成物 1

HCID 20497350Bis(p-aminocyclohexyl)methane phthalamide収率 28%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Bis(p-aminocyclohexyl)methane phthalamide was prepared by the aqueous reaction of bis(p-aminocyclohexyl)methane with phthalimide, according to a procedure similar to that published by Spring and Woods noted hereinabove. Thus, an emulsion of the amine in water was made using vigorous stirring. Phthalimide (1.0 mole per 2.4 moles of amine) was finely grounded and added to the emulsion at room temperature within a 10-minute period. The mixture was stirred for an additional 40 minutes and poured into a separatory funnel and extracted with chloroform. The chloroform solution was dried over magnesium sulfate, filtered and stripped. The product was washed with hexane and with anhydrous ethyl ether and then stripped in a vacuum oven.

後処理

  1. additionadded to the emulsion at room temperature within a 10-minute period
  2. additionpoured into a separatory funnel
  3. extractionextracted with chloroform
  4. dry with materialThe chloroform solution was dried over magnesium sulfate
  5. filtrationfiltered
  6. washThe product was washed with hexane and with anhydrous ethyl ether

出典と根拠

ORDレコード
ord-5822d7cb160f442cbccdc950b03a82a4
出典データセット
uspto-grants-1983_06
特許番号
US04390679

関連ノート

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