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

Sodium Hydroxide → (4-((3-Chloro-4-methoxybenzyl)amino)-2-(methylthio)pyrimidin-5-yl)methanol

HRID 1352742
ノート
印刷プレビュー

反応式

HRID 1352742 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][S:8][C:9]1[N:14]=[C:13]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[C:19]([Cl:25])[CH:18]=2)[C:12]([C:26](OCC)=[O:27])=[CH:11][N:10]=1.[OH-].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>O1CCCC1.O>[CH3:7][S:8][C:9]1[N:14]=[C:13]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[C:19]([Cl:25])[CH:18]=2)[C:12]([CH2:26][OH:27])=[CH:11][N:10]=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 14798Sodium HydroxideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 21226445Aluminium lithium hydrideHCID 22025927Ethyl 4-((3-chloro-4-methoxybenzyl)amino)-2-(methylsulfanyl)pyrimidine-5-carboxylate

生成物 1

HCID 22025932(4-((3-Chloro-4-methoxybenzyl)amino)-2-(methylthio)pyrimidin-5-yl)methanol

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
2 回
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of lithium aluminium hydride 4.15 g in tetrahydrofuran 150 ml is added a solution of 2-methylthio-4-(3-chloro-4-methoxybenzylamino)-5-ethoxycarbonylpyrimidine (prepared in Example 67-(1)) 38.32 g in tetrahydrofuran 100 ml at 5–10° C. under ice cooling over a period of 1 hour. After addition the mixture is stirred for a hour without an ice bath. Water 4.15 ml is added under ice cooling thereto, followed by addition of 3N aqueous sodium hydroxide solution 4.15 ml. To the mixture is added water 4.15 ml three times and the mixture is stirred at room temperature for 1 hour. After treating with magnesium sulfate and filtration, the resulting cake-like substances are washed with terahydrofuran. The filtrate is concentrated in vacuo and triturated with ethyl acetate-isopropyl ether. The resulting crystals are filtered and washed well with isopropyl-ether to give 2-methylthio-4-(3-chloro-4-methoxybenzylamino)-5-hydroxymethylpyrimidine as a pale yellow crystalline powder.

後処理

  1. additionAfter addition the mixture
  2. stirringthe mixture is stirred at room temperature for 1 hour
  3. washthe resulting cake-like substances are washed with terahydrofuran
  4. concentrationThe filtrate is concentrated in vacuo
  5. customtriturated with ethyl acetate-isopropyl ether
  6. filtrationThe resulting crystals are filtered
  7. washwashed well with isopropyl-ether

出典と根拠

ORDレコード
ord-8a46d2f9b0334e9fb38bb7b218e06258
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07220736B2

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