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Ammonia → HCID 70546830, 화합물

HRID 2059102
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HRID 2059102 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.[CH2:36]([NH2:43])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1.N>>[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:43][CH2:36][C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)[N:6]=1
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참가 물질

4

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HCID 222AmmoniaHCID 7504BenzylamineHCID 867383042,4-Bis{2-hydroxy-N-(2,2,6,6-tetramethyl-4-piperidyl)ethylamino}-6-chloro-1,3,5-triazine

생성물 1

HCID 70546830HCID 70546830, 화합물

실험 절차

2,4-Bis{2-hydroxy-N-(2,2,6,6-tetramethyl-4-piperidyl)ethylamino}-6-chloro-1,3,5-triazine (5.0 g) was reacted with benzylamine (25.0 g) for 8 hours and 30 minutes at 150°-160° C. The reaction mixture was poured into an aqueous ammonia solution, extracted with chloroform and dried over anhydrous potassium carbonate and chloroform was distilled off. The resulting residue was treated with silica gel chromatography (eluent=ethyl acetate:triethylamine:ethanol=10:12:3) to yield crystals, which were recrystallized from cyclohexane to afford the desired product as white crystals melting at 88° C.

후처리

  1. extractionextracted with chloroform
  2. dry with materialdried over anhydrous potassium carbonate and chloroform
  3. distillationwas distilled off
  4. additionThe resulting residue was treated with silica gel chromatography (eluent=ethyl acetate:triethylamine:ethanol=10:12:3)
  5. customto yield crystals, which
  6. customwere recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-0a002508f5b7495599f20274e310b52e
출처 데이터셋
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04321374

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