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

Methanesulfonic Acid → 2-Hydroxymethyl-4-methyl-8-[2'-(1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8dihydro-6H-pyrido[2,3-d]pyrimidin-7-one

HRID 129012
ノート
印刷プレビュー

反応式

HRID 129012 の反応式
[OH:1][CH2:2][C:3]1[N:4]=[C:5]([CH3:36])[C:6]2[CH2:12][CH2:11][C:10](=[O:13])[N:9]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[C:27]4[N:31](C(C)(C)C)[N:30]=[N:29][N:28]=4)=[CH:17][CH:16]=3)[C:7]=2[N:8]=1.CS(O)(=O)=O>C1(C)C=CC=CC=1>[OH:1][CH2:2][C:3]1[N:4]=[C:5]([CH3:36])[C:6]2[CH2:12][CH2:11][C:10](=[O:13])[N:9]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[C:27]4[NH:31][N:30]=[N:29][N:28]=4)=[CH:17][CH:16]=3)[C:7]=2[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

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 193729942-Hydroxymethyl-4-methyl-8-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one

生成物 1

HCID 1784330362-Hydroxymethyl-4-methyl-8-[2'-(1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8dihydro-6H-pyrido[2,3-d]pyrimidin-7-one収率 102.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 2-hydroxymethyl-4-methyl-8-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one (1.2 g, 2.50 mmol), methanesulfonic acid (2.40 g, 25.0 mmol), and toluene (14 mL) was heated under reflux for 20 h. The mixture was concentrated, taken up in water, and the pH was adjusted to 7-8 with 1 N NaOH. The aqueous mixture was extracted with EtOAc (discarded), acidified to pH 4 with 1N HCl, and extracted with CHCl3. The CHCl3 layers were dried (MgSO4) and concentrated to give 1.10 g of a foam. Trituration with EtOAc/acetone and recrystallization from EtOH gave 0.45 g (46%) of product as a white solid, mp 218°-220° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 20 h
  3. concentrationThe mixture was concentrated
  4. extractionThe aqueous mixture was extracted with EtOAc (discarded)
  5. extractionextracted with CHCl3
  6. dry with materialThe CHCl3 layers were dried (MgSO4)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-ed341cdad0434248b3e7cdf6232a16cd
出典データセット
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05466692

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