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

4-Toluenesulfonyl chloride → (S)-tert-Butyl 2-((tosyloxy)methyl)morpholine-4-carboxylate

HRID 706967
ノート
印刷プレビュー

反応式

HRID 706967 の反応式
[OH:1][CH2:2][C@H:3]1[O:8][CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1.C(N(CC)CC)C.[CH3:23][C:24]1[CH:29]=[CH:28][C:27]([S:30](Cl)(=[O:32])=[O:31])=[CH:26][CH:25]=1>ClCCl.[Cl-].[Na+].O>[S:30]([O:1][CH2:2][C@H:3]1[O:8][CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1)([C:27]1[CH:28]=[CH:29][C:24]([CH3:23])=[CH:25][CH:26]=1)(=[O:32])=[O:31]
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 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 1512577tert-Butyl (2S)-2-(hydroxymethyl)morpholine-4-carboxylate

生成物 1

HCID 54043638(S)-tert-Butyl 2-((tosyloxy)methyl)morpholine-4-carboxylate

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回
HCID 57417360
Sodium chloride; water
溶媒

実験手順

To a solution of (S)-tert-butyl 2-(hydroxymethyl)morpholine-4-carboxylate (1 g) in dichloromethane (50 mL) was added triethylamine (1.604 mL) and 4-methylbenzene-1-sulfonyl chloride (1.097 g). The mixture was stirred at ambient temperature under nitrogen for 72 hours. The reaction was diluted with methylene chloride (50 mL) and brine (100 mL). The brine layer was extracted with methylene chloride (75 mL). The combined organics were dried over sodium sulfate, filtered and concentrated. The crude material was purified on a silica gel column eluting with a 15-65% ethyl acetate in hexane gradient to provide the title compound.

後処理

  1. extractionThe brine layer was extracted with methylene chloride (75 mL)
  2. dry with materialThe combined organics were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude material was purified on a silica gel column
  6. washeluting with a 15-65% ethyl acetate in hexane gradient

出典と根拠

ORDレコード
ord-435583a5ceb14ddb9c313e5166b076e0
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09174982B2

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