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

Triethylamine → [3-Methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-(8-methyl-8-phenyl-5,6,7,8-tetrahydro-quinazolin-2-yl)-amine

HRID 2076043
ノート
印刷プレビュー

反応式

HRID 2076043 の反応式
CN(C)[CH:3]=[C:4]1[C:9](=O)[C:8]([CH3:17])([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6][CH2:5]1.[N+]([O-])(O)=O.[N+]([O-])(O)=O.[CH3:27][O:28][C:29]1[CH:30]=[C:31]([NH:41][C:42]([NH2:44])=[NH:43])[CH:32]=[CH:33][C:34]=1[N:35]1[CH:39]=[C:38]([CH3:40])[N:37]=[CH:36]1.C(N(CC)CC)C>C(O)C.C(OCC)(=O)C>[CH3:27][O:28][C:29]1[CH:30]=[C:31]([NH:41][C:42]2[N:44]=[CH:3][C:4]3[CH2:5][CH2:6][CH2:7][C:8]([CH3:17])([C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=4)[C:9]=3[N:43]=2)[CH:32]=[CH:33][C:34]=1[N:35]1[CH:39]=[C:38]([CH3:40])[N:37]=[CH:36]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 670961136-[1-Dimethylamino-methylidene]-2-methyl-2-phenylcyclohexanoneHCID 178493228HCID 178493228、化合物

生成物 1

HCID 57780701[3-Methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-(8-methyl-8-phenyl-5,6,7,8-tetrahydro-quinazolin-2-yl)-amine収率 19%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 6-[1-dimethylamino-methylidene]-2-methyl-2-phenylcyclohexanone (103 mg, 0.42 mmol), N-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-guanidine dinitrate (157 mg, 0.42 mmol), and triethylamine (0.29 mL, 2.1 mmol) in ethanol (1 mL) was heated at reflux for 18 h. The mixture was cooled, diluted with ethyl acetate (30 mL) and then washed with saturated aqueous sodium carbonate solution (10 mL) and with brine (10 mL). The organic layer was dried over sodium sulfate and evaporated under reduced pressure. The residual material was purified by column chromatography on silica gel using dichloromethane/methanol (20:1 v/v) as eluent to give the title compound (34 mg, 19%). MS ISP (m/e): 426.1 [(M+H)+]. mp 207-209° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 18 h
  3. temperatureThe mixture was cooled
  4. washwashed with saturated aqueous sodium carbonate solution (10 mL) and with brine (10 mL)
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customThe residual material was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-2514d2d141dc403fb668673ba5b938a0
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07923450B2

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