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Sodium Hydroxide → 2-(2-Trityloxycarbamoyl-ethyl)-succinic acid 4-tert-butyl ester

HRID 902929
ノート
印刷プレビュー

反応式

HRID 902929 の反応式
C[O:2][C:3](=[O:38])[CH:4]([CH2:13][CH2:14][C:15](=[O:37])[NH:16][O:17][C:18]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:5][C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7].[OH-].[Na+]>CO.O>[C:9]([O:8][C:6](=[O:7])[CH2:5][CH:4]([CH2:13][CH2:14][C:15](=[O:37])[NH:16][O:17][C:18]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:3]([OH:38])=[O:2])([CH3:12])([CH3:10])[CH3:11]
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 14798Sodium HydroxideHCID 131725937HCID 131725937、化合物

生成物 1

HCID 877349892-(2-Trityloxycarbamoyl-ethyl)-succinic acid 4-tert-butyl ester

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

To a solution of the compound of example 65 (2.27 g, 4.39 mmol) in a mixture of methanol/water (4:1, 50 mL) was added a solution of sodium hydroxide (1N, 9 mL). The resulting mixture was stirred for 24 h at room temperature. The solvent was evaporated and the residue was partitioned between water and ether. The alkaline phase acidified using HCl (6N) and extracted with ethyl acetate followed by drying over sodium sulfate, filtration and evaporation. The product was converted to an off-white foam under high vacuum. 1H-NMR(CDCl3, 400 MHz: 1.42(s, 9H); 1.59(m, 3H); 1.88-2.54(m, 4H); 7.33(m, 15H); 7.46(s, broad, 1H).

後処理

  1. customThe solvent was evaporated
  2. customthe residue was partitioned between water and ether
  3. extractionextracted with ethyl acetate
  4. dry with materialby drying over sodium sulfate, filtration and evaporation

出典と根拠

ORDレコード
ord-8de34138c0a44a3d942235bafa23c9c2
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07365091B2

反応ノート

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