ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1,4-Benzenedimethanamine → HCID 86738306、化合物

HRID 2059104
ノート
印刷プレビュー

反応式

HRID 2059104 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.[C:36]1([CH2:44][NH2:45])[CH:41]=[CH:40][C:39]([CH2:42][NH2:43])=[CH:38][CH:37]=1>C1(C)C(C)=CC=CC=1>[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][CH2:42][C:39]2[CH:40]=[CH:41][C:36]([CH2:44][NH:45][C:7]3[N:8]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]4[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:23])([CH3:24])[CH2:16]4)[OH:14])[N:10]=[C:5]([NH:4][CH2:3][CH:2]([CH:26]4[CH2:27][C:28]([CH3:35])([CH3:34])[NH:29][C:30]([CH3:33])([CH3:32])[CH2:31]4)[OH:1])[N:6]=3)=[CH:37][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 2

HCID 683151,4-BenzenedimethanamineHCID 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 86738306HCID 86738306、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

2,4-Bis{2-hydroxy-N-(2,2,6,6-tetramethyl-4-piperidyl)ethylamino}-6-chloro-1,3,5-triazine (15.4 g) and p-xylylenediamine (1.4 g) were dissolved in xylene (50 ml) and the solution was heated to reflux for 5 hours. The reaction mixture was poured into ice water. After saturation with potassium carbonate, the mixture was extracted with a mixture of benzene (300 ml) and chloroform (500 ml). The extract was dried over anhydrous potassium carbonate and benzene and chloroform were distilled off. The resulting residue was treated with silica gel column chromatography (eluent=ethyl acetate:triethylamine:ethanol=3:1:1) to yield crystals, which were recrystallized from cyclohexane to give the desired product with a melting point of 151°-156° C.

後処理

  1. temperaturethe solution was heated
  2. temperatureto reflux for 5 hours
  3. extractionAfter saturation with potassium carbonate, the mixture was extracted with a mixture of benzene (300 ml) and chloroform (500 ml)
  4. dry with materialThe extract was dried over anhydrous potassium carbonate and benzene and chloroform
  5. distillationwere distilled off
  6. additionThe resulting residue was treated with silica gel column chromatography (eluent=ethyl acetate:triethylamine:ethanol=3:1:1)
  7. customto yield crystals, which
  8. customwere recrystallized from cyclohexane

出典と根拠

ORDレコード
ord-501d09a5556148c89bce40828176d416
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

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート