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Diethylenetriaminepentaacetic acid → Diethylenetriaminepentaacetic dianhydride

HRID 2211208
ノート
印刷プレビュー

反応式

HRID 2211208 の反応式
[CH2:1]([N:12]([CH2:24][C:25]([OH:27])=[O:26])[CH2:13][CH2:14][N:15]([CH2:20][C:21]([OH:23])=O)[CH2:16][C:17]([OH:19])=[O:18])[CH2:2][N:3]([CH2:8][C:9]([OH:11])=[O:10])[CH2:4][C:5]([OH:7])=O.C(OC(=O)C)(=O)C>N1C=CC=CC=1>[CH2:20]1[N:15]([CH2:14][CH2:13][NH+:12]([CH2:24][C:25]([O-:27])=[O:26])[CH2:1][CH2:2][N:3]2[CH2:8][C:9](=[O:10])[O:11][C:5](=[O:7])[CH2:4]2)[CH2:16][C:17](=[O:19])[O:18][C:21]1=[O:23]
参加物実験手順出典と根拠反応ノート

参加物

4

反応物 2

HCID 3053Diethylenetriaminepentaacetic acidHCID 7918Acetic Anhydride

生成物 1

HCID 16760401Diethylenetriaminepentaacetic dianhydride

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

DTPA (78.6 g.) was heated to about 70° C. with a mixture of acetic anhydride (75.6 ml) and anhydrous pyridine (102.2 ml) for 18 hours and 65.9 g. of diethylenetriamine pentaacetic acid dianhydride ("DTPADA") was obtained. DTPADA (64.3 g.) was then heated with an excess of 2,6-dimethylaniline (50.2 g) in anhydrous pryridine (1200 ml) and refluxed at a temperature of about 115° C. for 2 hours. The reaction mixture was then cooled and added to 1500 ml of ethyl acetate. The resulting mixture was chilled for about 16 hours to a temperature of about 4° C. The precipitate was collected, washed with ethyl acetate and dried under vacuum at 97° C. and 0.5 mm for about 16 hours. About 59.8 g of N,N"-bis (2,6-dimethylcarbaniloylmethylene) diethylenetriamine triacetic acid ("DTPA-bis 2,6-dimethylaniline") was obtained as the monohydrate. The melting point was determined to be 195°-199° C. and elemental analysis determined for C30H43N5O9 was 58.4% C, 6.76% H, and 11.22% N.

出典と根拠

ORDレコード
ord-e251e9b3f2104212b1578bcf86a865a0
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05463030

反応ノート

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