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Phosphorous acid → 1,4,7-Triazacyclononane

HRID 22464
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HRID 22464 반응식
[CH2:1]1[NH:9][CH2:8][CH2:7][NH:6][CH2:5][CH2:4][NH:3][CH2:2]1.[CH2:10]1[CH2:21][NH:20][CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14][CH2:13][NH:12][CH2:11]1.[P:22](O)([OH:24])[OH:23]>>[CH2:1]1[NH:9][CH2:8][CH2:7][NH:6][CH2:5][CH2:4][NH:3][CH2:2]1.[CH2:7]([O:24][PH:22]([CH2:19][CH:18]=[CH2:17])=[O:23])[CH3:8].[CH2:18]1[CH2:17][NH:16][CH2:15][CH2:14][CH2:13][NH:12][CH2:11][CH2:10][CH2:21][NH:20][CH2:19]1
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참가 물질

6

반응물 3

HCID 107909Phosphorous acidHCID 1883181,4,7-TriazacyclononaneHCID 4707781,5,9-Triazacyclododecane

생성물 3

HCID 1883181,4,7-TriazacyclononaneHCID 4707781,5,9-TriazacyclododecaneHCID 178460680HCID 178460680, 화합물

실험 절차

It appears however that the HI3 salts of the monomethylenesulfonic acids of [9]aneN3 and [12]aneN3 can be used directly. When these trilodide salts are added to melted phosphorous acid at 80° C., at 25° C., HP(=O)Et(OEt), or HP(=O)(OEt)2, a very exothermic reaction occurs whereby the respective monomethylenephosphonate, the monomethylene(ethyl)-phosphinate ethyl ester and the monomethylenephosphonate diethyl ester of [9]aneN3 (FIGS. 31A, 31B, and 31C) and the monomethylenephosphonate diethyl ester and the monomethylene(ethyl)-phosphinate ethyl ester of [12]aneN3 (FIGS. 32A and 32B) are formed almost quantitatively within a few seconds.

후처리

  1. additionWhen these trilodide salts are added
  2. customat 80° C.
  3. customat 25° C., HP(=O)Et(OEt), or HP(=O)(OEt)2, a very exothermic reaction

출처 및 근거

ORD 기록
ord-c7dec6c7de3e4f5bbe8bd04851220980
출처 데이터셋
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05428155

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