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Diethylenetriaminepentaacetic acid → Diethylenetriaminepentaacetic dianhydride

HRID 2211208
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HRID 2211208 반응식
[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]
참가 물질실험 절차출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3053Diethylenetriaminepentaacetic acidHCID 7918Acetic Anhydride

생성물 1

HCID 16760401Diethylenetriaminepentaacetic dianhydride

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

출처 및 근거

ORD 기록
ord-e251e9b3f2104212b1578bcf86a865a0
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05463030

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