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Water → (2S,4S)-2-mesyloxymethyl-N-(p-nitrobenzyloxycarbonyl)-4-tritylthiopyrrolidine

HRID 1034479
ノート
印刷プレビュー

反応式

HRID 1034479 の反応式
[N+:1]([C:4]1[CH:40]=[CH:39][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:16][C@@H:15]([S:17][C:18]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14][C@H:13]2[CH2:37][OH:38])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(N(CC)CC)C.[CH3:48][S:49](Cl)(=[O:51])=[O:50].O>ClCCl>[CH3:48][S:49]([O:38][CH2:37][C@@H:13]1[CH2:14][C@H:15]([S:17][C:18]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH2:16][N:12]1[C:10]([O:9][CH2:8][C:7]1[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:40][CH:39]=1)=[O:11])(=[O:51])=[O:50]
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 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 15056118(2S,4S)-2-hydroxymethyl-N-(p-nitrobenzyloxycarbonyl)-4-tritylthiopyrrolidine

生成物 1

HCID 15056119(2S,4S)-2-mesyloxymethyl-N-(p-nitrobenzyloxycarbonyl)-4-tritylthiopyrrolidine収率 85.2%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of (2S,4S)-1-p-nitrobenzyloxycarbonyl-4-tritylthiopyrrolidine-2-methanol (5.0 g: 9.01 mmole) in dichloromethane (50 ml) stirring at -15° C., triethylamine (1.63 ml: 1.3 eq.) and methanesulfonyl chloride (0.85 ml: 1.1 eq.) are added. The mixture is stirred at -15° to -10° C. for 30 minutes. The reaction mixture is poured into water and extracted with dichloromethane. The extract is successively washed with dilute hydrochloric acid, aqueous sodium hydrogen carbonate, and water, dried over magnesium sulfate, and concentrated in vacuo. The residue is purified by silica gel column chromatography (toluene: ethyl acetate=9:1) to give (2S,4S)-1-p-nitrobenzyloxycarbonyl-4-tritylthiopyrrolidine-2-methanol methanesulfonate (4.86 g). Yield: 85.2%. NMR δ(CDCl3) ppm: 1.65 to 1.93(m, 1H), 2.00 to 2.26(m, 1H), 2.68 to 2.92(m, 3H), 2.96(s, 3H), 3.78 to 3.98(m, 1H), 4.16 to 4.30(m, 1H), 4.38 to 4.52(m, 1H), 5.11(br s, 2H), 7.08 to 7.52(m, 17H), 8.24(d, J=9 Hz, 2H). IR ν (CHCl3) cm-1 : 1699, 1606.

後処理

  1. extractionextracted with dichloromethane
  2. washThe extract is successively washed with dilute hydrochloric acid, aqueous sodium hydrogen carbonate, and water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by silica gel column chromatography (toluene: ethyl acetate=9:1)

出典と根拠

ORDレコード
ord-94771a4468d641b28e1ce1a380baa10e
出典データセット
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05317016

反応ノート

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