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Ammonia → HCID 70546830、化合物

HRID 2059102
ノート
印刷プレビュー

反応式

HRID 2059102 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

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

生成物 1

HCID 70546830HCID 70546830、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0a002508f5b7495599f20274e310b52e
出典データセット
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04321374

反応ノート

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