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Triethyl 2,2',2''-(1,4,7,10-tetraazacyclododecane-1,4,7-triyl)triacetate → HCID 67600263, 화합물

HRID 580767
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HRID 580767 반응식
[CH2:1]([O:3][C:4]([CH2:6][N:7]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14][N:13]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:12][CH2:11][N:10]([CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH2:9][CH2:8]1)=[O:5])[CH3:2].[CH3:31][C:32]1([CH3:43])[O:36][CH2:35][CH:34]([CH2:37][NH:38][S:39]([CH3:42])(=[O:41])=[O:40])[O:33]1>C(O)C>[CH3:31][C:32]1([CH3:43])[O:36][CH2:35][CH:34]([CH2:37][N:38]([S:39]([CH3:42])(=[O:40])=[O:41])[CH2:31][CH:32]([OH:33])[CH2:43][N:16]2[CH2:15][CH2:14][N:13]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:12][CH2:11][N:10]([CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH2:9][CH2:8][N:7]([CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH2:18][CH2:17]2)[O:33]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10906130Triethyl 2,2',2''-(1,4,7,10-tetraazacyclododecane-1,4,7-triyl)triacetateHCID 54158307HCID 54158307, 화합물

생성물 1

HCID 67600263HCID 67600263, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

200 ml of absolute ethanol is poured over 8.61 g (20 mmol) of N,N',N"-tris-(ethoxycarbonylmethyl)-1,4,7,10-tetraazacyclododecane (produced according to DE 36 25 417 A1) in a bomb tube. After 5.31 g (20 mmol) of N-[(3,3-dimethyl-2,4-dioxa-cyclopentyl)-methyl]-methanesulfonic acid amide is added (Example 21), the bomb tube is closed, flushed with nitrogen, and the resulting reaction mixture is heated for 16 hours to 90° C. After the reaction (TLC control) is completed, the solvent is evaporated in a vacuum and the yellowish, oily residue is chromatographed on silica gel (eluent: chloroform/methanol; methanol: 0-80%).

후처리

  1. customthe bomb tube is closed
  2. customflushed with nitrogen
  3. customthe resulting reaction mixture
  4. temperatureis heated for 16 hours to 90° C
  5. customAfter the reaction (TLC control)
  6. customthe solvent is evaporated in a vacuum
  7. customthe yellowish, oily residue is chromatographed on silica gel (eluent: chloroform/methanol; methanol: 0-80%)

출처 및 근거

ORD 기록
ord-466d0477b74f4d6795123b05ab9634b5
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05919431

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