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

Diisopropylethylamine → 4-(3-chloro-4-methoxybenzyloxy)-2-(methylmercapto)-N-(pyrimidin-2-ylmethyl)pyrimidin e-5-carboxamide

HRID 874509
ノート
印刷プレビュー

反応式

HRID 874509 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[CH2:5][O:6][C:7]1[C:12]([C:13]([OH:15])=O)=[CH:11][N:10]=[C:9]([S:16][CH3:17])[N:8]=1.CCN(C(C)C)C(C)C.CN(C(O[N:40]1N=[N:47][C:42]2[CH:43]=[CH:44][CH:45]=[N:46][C:41]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.N1C=CC=NC=1CN>C1COCC1.O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[CH2:5][O:6][C:7]1[C:12]([C:13]([NH:47][CH2:42][C:41]2[N:40]=[CH:43][CH:44]=[CH:45][N:46]=2)=[O:15])=[CH:11][N:10]=[C:9]([S:16][CH3:17])[N:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 46580472-PyrimidinemethanamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 712350394-(3-chloro-4-methoxybenzyloxy)-2-(methylmercapto)pyrimidine-5-carboxylic Acid

生成物 1

HCID 71235035
4-(3-chloro-4-methoxybenzyloxy)-2-(methylmercapto)-N-(pyrimidin-2-ylmethyl)pyrimidin e-5-carboxamide
収率 16%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

4-(3-chloro-4-methoxybenzyloxy)-2-(methylmercapto)pyrimidine-5-carboxylic acid (300 mg, 0.88 mmol), DIEA (0.5 mL, 2.88 mmol) were dissolved in 30 mL of THF, HATU (405 mg, 1.06 mmol) and pyrimidin-2-ylmethylamine (115 mg, 1.06 mmol) were added under ice-water-bath, reacted at room temperature overnight, to the reaction solution was added 100 mL of water, then extracted with dichloromethane, dried with anhydrous sodium sulfate, dried by rotation, then solid was separated with silica gel column (dichloromethane:methanol=40:1) to obtain a white solid 4-(3-chloro-4-methoxybenzyloxy)-2-(methylmercapto)-N-(pyrimidin-2-ylmethyl)pyrimidine-5-carboxamide 60 mg, yield 16%.

後処理

  1. customreacted at room temperature overnight, to the reaction solution
  2. extractionextracted with dichloromethane
  3. dry with materialdried with anhydrous sodium sulfate
  4. customdried by rotation
  5. customsolid was separated with silica gel column (dichloromethane:methanol=40:1)

出典と根拠

ORDレコード
ord-7dcf218bcd5b4ae48a246240ce0e5301
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08980904B2

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