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

Acetic Acid → HCID 178482059、化合物

HRID 1851305
ノート
印刷プレビュー

反応式

HRID 1851305 の反応式
[NH:1]1[CH2:4][CH:3]([C:5]2[NH:9][N:8]=[C:7]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=3)[N:6]=2)[CH2:2]1.C(N(CC)CC)C.[CH3:23][NH:24][C:25]1[N:30]2[CH:31]=[CH:32][N:33]=[C:29]2[N:28]=[C:27]([C:34]2[CH:41]=[CH:40][C:37]([CH:38]=O)=[CH:36][CH:35]=2)[C:26]=1[C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1.C(O)(=O)C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C([O-])(O)=O.[Na+]>CN1C(=O)CCC1>[CH3:23][NH:24][C:25]1[N:30]2[CH:31]=[CH:32][N:33]=[C:29]2[N:28]=[C:27]([C:34]2[CH:41]=[CH:40][C:37]([CH2:38][N:1]3[CH2:4][CH:3]([C:5]4[N:6]=[C:7]([C:10]5[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=5)[NH:8][N:9]=4)[CH2:2]3)=[CH:36][CH:35]=2)[C:26]=1[C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 176Acetic AcidHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 687522842-(5-Azetidine-3-yl-[1,2,4]triazole-3-yl)-pyridineHCID 866306614-(5-Methylamino-6-phenyl-imidazo[1,2-a]pyrimidin-7-yl)-benzaldehyde

生成物 1

HCID 178482059
HCID 178482059、化合物
収率 37.3%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

257 mg (0.94 mmol) 2-(5-Azetidine-3-yl-[1,2,4]triazole-3-yl)-pyridine×2HCl are dissolved in 7.3 mL NMP. After addition of 0.26 mL (1.88 mmol) triethylamine the reaction mixture is stirred for one hour. 280 mg (0.85 mmol) 4-(5-Methylamino-6-phenyl-imidazo[1,2-a]pyrimidin-7-yl)-benzaldehyde and 0.12 mL (2.05 mmol) acetic acid are added. The reaction mixture is stirred for 24 hours at room temperature. 469.9 mg (2.2 mmol) NaBH(OAc)3, are added in portions and the reaction mixture is stirred at room temperature over night. The reaction mixture is treated with saturated NaHCO3. The precipitate is filtered off, washed with water, dried and purified by chromatography (silicagel, eluents: dichloromethane/methanol) yielding 163 mg (33.5%) of the desired title compound.

後処理

  1. stirringThe reaction mixture is stirred for 24 hours at room temperature
  2. stirringthe reaction mixture is stirred at room temperature over night
  3. filtrationThe precipitate is filtered off
  4. washwashed with water
  5. customdried
  6. custompurified by chromatography (silicagel, eluents: dichloromethane/methanol)

出典と根拠

ORDレコード
ord-bdd0c5f4271c424b8d2bc6436e67f9e4
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08957064B2

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