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

Pyridine → HCID 70171875、化合物

HRID 2229753
ノート
印刷プレビュー

反応式

HRID 2229753 の反応式
[C:1]([NH:4][C:5]1[CH:19]=[CH:18][N:8]([C@@H:9]2[O:16][C@H:13]([CH2:14][OH:15])[C@@H:11]([OH:12])[C@H:10]2[F:17])[C:7](=[O:20])[N:6]=1)(=[O:3])[CH3:2].N1C=CC=CC=1.[CH3:27][O:28][C:29]1[C:30]([O:49][CH3:50])=[C:31]([CH:46]=[CH:47][CH:48]=1)[C:32](Cl)([C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1>CN(C)C1C=CN=CC=1.CO>[CH3:27][O:28][C:29]1[C:30]([O:49][CH3:50])=[C:31]([CH:46]=[CH:47][CH:48]=1)[C:32]([O:15][CH2:14][C@H:13]1[O:16][C@@H:9]([N:8]2[CH:18]=[CH:19][C:5]([NH:4][C:1](=[O:3])[CH3:2])=[N:6][C:7]2=[O:20])[C@H:10]([F:17])[C@@H:11]1[OH:12])([C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1)[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 1049PyridineHCID 22094552N-Acetyl-2'-deoxy-2'-fluorocytidineHCID 66624882Dimethoxytrityl chloride

生成物 1

HCID 70171875HCID 70171875、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 887Methanol溶媒

実験手順

4 mmol of 4-N-acetyl-2′-fluoro-2′-deoxycytidine are taken up in 25 ml of abs. pyridine in a 100 ml Schlenk flask and, at room temperature, 1.3 g (about 4.4 mmol) of dimethoxytrityl chloride and 20 mg of 4-dimethylaminopyridine are added. After three hours, 1 ml of methanol was added to the mixture, which was then evaporated to dryness in vacuo. The remaining oil is taken up in 50 ml of methylene chloride (deacidified over aluminum oxide) and extracted three times with 50 ml of water. The organic phase is dried over sodium sulfate. After the methylene chloride had been stripped off, the crude product remained as solid foam. The crude product is purified by chromatography on silica gel 60H (column 2×20 cm, mobile phase methylene chloride with 0.1% pyridine, gradient methanol). The product was eluted with 3% methanol in methylene chloride. After the solvent has been stripped off, 1.39 g (59% of theory) of a white foamy solid remain.

後処理

  1. customwas then evaporated to dryness in vacuo
  2. extractionextracted three times with 50 ml of water
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customThe crude product is purified by chromatography on silica gel 60H (column 2×20 cm, mobile phase methylene chloride with 0.1% pyridine, gradient methanol)
  5. washThe product was eluted with 3% methanol in methylene chloride

出典と根拠

ORDレコード
ord-19559ed652ea4cafbd131193eceb8dcb
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06420546B1

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