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 Chloride → [4-(2-Hydroxymethylmorpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetic acid ethyl ester

HRID 2278550
ノート
印刷プレビュー

反応式

HRID 2278550 の反応式
[CH2:1]([O:3][C:4](=[O:14])[CH2:5][C:6]1[NH:7][C:8](=[O:13])[CH:9]=[C:10](Cl)[N:11]=1)[CH3:2].Cl.[NH:16]1[CH2:21][CH2:20][O:19][CH:18]([CH2:22][OH:23])[CH2:17]1.[Na+].[Cl-].C(Cl)Cl>CS(C)=O.C(N(CC)CC)C.C(OC(C)C)(C)C>[CH2:1]([O:3][C:4](=[O:14])[CH2:5][C:6]1[NH:7][C:8](=[O:13])[CH:9]=[C:10]([N:16]2[CH2:21][CH2:20][O:19][CH:18]([CH2:22][OH:23])[CH2:17]2)[N:11]=1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 5234Sodium ChlorideHCID 6344DichloromethaneHCID 19777263Morpholin-2-ylmethanol hydrochlorideHCID 136378677Ethyl 2-(6-chloro-4-oxo-1,4-dihydropyrimidin-2-yl)acetate

生成物 1

HCID 136378679[4-(2-Hydroxymethylmorpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetic acid ethyl ester収率 14%

試薬・触媒・溶媒 3

HCID 679
Dimethyl Sulfoxide
溶媒
HCID 7914Diisopropyl Ether溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
85 °C

実験手順

Under argon, in a 500 ml round-bottomed flask equipped with a thermometer and a condenser, 10 g of (4-chloro-6-oxo-1,6-dihydropyrimidin-2-yl)acetic acid ethyl ester (example 25b, step 5b) and 9.6 g of morpholin-2-yl-methanol hydrochloride obtained previously are successively placed in 200 ml of DMSO and 16.1 ml of triethylamine. The reaction medium is heated for 22 h at 85° C. After returning to ambient temperature (20° C.), the reaction medium is poured into a saturated NaCl solution, and the mixture is extracted with 8×250 ml of ethyl acetate. The organic extracts are combined, dried over magnesium sulfate, filtered, and evaporated under reduced pressure. A solid is obtained which is slurried in diisopropyl ether containing 10% of methylene chloride. The solid is filtered off, and rinsed twice and then once with pentane. [4-(2-Hydroxymethylmorpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetic acid ethyl ester is isolated (1.9 g; yield=14%) in the form of a beige solid.

後処理

  1. customobtained previously
  2. customAfter returning to ambient temperature
  3. custom(20° C.)
  4. extractionthe mixture is extracted with 8×250 ml of ethyl acetate
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customA solid is obtained which
  9. filtrationThe solid is filtered off
  10. washrinsed twice

出典と根拠

ORDレコード
ord-7e4def9c85e048c18b2ba576db104ce2
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133168B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート