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Triethylenetetramine → HCID 86738307, 화합물

HRID 2059105
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HRID 2059105 반응식
[OH:1][CH:2]([CH:26]1[CH2:31][C:30]([CH3:33])([CH3:32])[NH:29][C:28]([CH3:35])([CH3:34])[CH2:27]1)[CH2:3][NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]2[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:24])([CH3:23])[CH2:16]2)[OH:14])[N:8]=[C:7](Cl)[N:6]=1.[NH2:36][CH2:37][CH2:38][NH:39][CH2:40][CH2:41][NH:42][CH2:43][CH2:44][NH2:45].[OH-:46].[Na+]>O1CCOCC1.O>[OH:1][CH:2]([CH:26]1[CH2:31][C:30]([CH3:33])([CH3:32])[NH:29][C:28]([CH3:35])([CH3:34])[CH2:27]1)[CH2:3][NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]2[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:24])([CH3:23])[CH2:16]2)[OH:14])[N:8]=[C:7]([NH:36][CH2:37][CH2:38][N:39]([C:7]2[N:8]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]3[CH2:16][C:17]([CH3:24])([CH3:23])[NH:18][C:19]([CH3:21])([CH3:22])[CH2:20]3)[OH:14])[N:10]=[C:5]([NH:4][CH2:3][CH:2]([CH:26]3[CH2:27][C:28]([CH3:35])([CH3:34])[NH:29][C:30]([CH3:33])([CH3:32])[CH2:31]3)[OH:1])[N:6]=2)[CH2:40][CH2:41][N:42]([C:7]2[N:8]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]3[CH2:16][C:17]([CH3:24])([CH3:23])[NH:18][C:19]([CH3:21])([CH3:22])[CH2:20]3)[OH:14])[N:10]=[C:5]([NH:4][CH2:3][CH:2]([CH:26]3[CH2:27][C:28]([CH3:35])([CH3:34])[NH:29][C:30]([CH3:33])([CH3:32])[CH2:31]3)[OH:1])[N:6]=2)[CH2:43][CH2:44][NH:45][C:7]2[N:8]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]3[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:23])([CH3:24])[CH2:16]3)[OH:46])[N:10]=[C:5]([NH:4][CH2:3][CH:2]([CH:26]3[CH2:27][C:28]([CH3:35])([CH3:34])[NH:29][C:30]([CH3:33])([CH3:32])[CH2:31]3)[OH:1])[N:6]=2)[N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 5565TriethylenetetramineHCID 14798Sodium HydroxideHCID 867383042,4-Bis{2-hydroxy-N-(2,2,6,6-tetramethyl-4-piperidyl)ethylamino}-6-chloro-1,3,5-triazine

생성물 1

HCID 86738307HCID 86738307, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 31275
1,4-Dioxane
용매

실험 절차

2,4-Bis{2-hydroxy-N-(2,2,6,6-tetramethyl-4-piperidyl)ethylamino}-6-chloro-1,3,5-triazine (8.0 g) and triethylenetetramine (0.5 g) were dissolved in dioxane (100 ml) and to the solution was added an aqueous solution of sodium hydroxide (0.7 g) in water (10 ml). The mixture was heated to reflux for 6 hours. Dioxane was distilled off from the reaction mixture and the residue was extracted with benzene. The extract was treated with silica gel column chromatography (eluent=ethyl acetate:benzene:ethanol:triethylamine=20:4:2:1) to give the desired product as white crystals melting at 158° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 6 hours
  3. distillationDioxane was distilled off from the reaction mixture
  4. extractionthe residue was extracted with benzene
  5. additionThe extract was treated with silica gel column chromatography (eluent=ethyl acetate:benzene:ethanol:triethylamine=20:4:2:1)

출처 및 근거

ORD 기록
ord-b27f0edc11d948079e1ba986925693d5
출처 데이터셋
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04321374

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