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Hydrogen chloride-ethyl acetate → HCID 178486643、化合物

HRID 1834198
ノート
印刷プレビュー

反応式

HRID 1834198 の反応式
[N:1]#[N:2].S(S(O)=O)(O)=O.C([O:13][C:14](=[O:52])[CH2:15][N:16]([C:24](=[O:51])[C@H:25]([CH2:44][CH2:45][CH2:46][NH:47][C:48](=[NH:50])[NH2:49])[NH:26][S:27]([C:30]1[CH:39]=[CH:38][C:37]2[C:32](=[CH:33][C:34]([O:42][CH3:43])=[C:35]([O:40][CH3:41])[CH:36]=2)[CH:31]=1)(=[O:29])=[O:28])[CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)(C)(C)C.Cl.C(OCC)(=O)C>C(Cl)(Cl)Cl>[N:1]#[N:2].[CH3:41][O:40][C:35]1[CH:36]=[C:37]2[C:32](=[CH:33][C:34]=1[O:42][CH3:43])[CH:31]=[C:30]([S:27]([NH:26][C@H:25]([C:24]([N:16]([CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:15][C:14]([OH:52])=[O:13])=[O:51])[CH2:44][CH2:45][CH2:46][NH:47][C:48](=[NH:49])[NH2:50])(=[O:29])=[O:28])[CH:39]=[CH:38]2
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 21866389Hydrogen chloride-ethyl acetateHCID 178486644HCID 178486644、化合物

生成物 1

HCID 178486643HCID 178486643、化合物収率 78.6%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 2.00 g of N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl-N-benzylglycine tert-butyl ester hydrosulfite in 20 ml of chloroform was added 50 ml of 15% HCl-ethyl acetate. The reaction mixture was stirred for 5 hours at room temperature. At the end of this period, the reaction mixture was evaporated to dryness. The residue was washed several times with dry diethyl ether and chromatographed on 80 ml of Daiaion® SK 102 ion exchange resin (200-300 mesh, H+ form, manufactured by Mitsubishi Chemical Industries Limited) packed in water, washed with water and eluted with 3% ammonium hydroxide solution. The fraction eluted from 3% ammonium hydroxide solution was evaporated to dryness to give 1.20 g (70 percent) of N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl-N-benzylglycine as an amorphous solid, I.R. (KBr): 3,370, 3,200, 1.615 cm-1.

後処理

  1. customAt the end of this period, the reaction mixture was evaporated to dryness
  2. washThe residue was washed several times with dry diethyl ether
  3. customchromatographed on 80 ml of Daiaion® SK 102 ion exchange resin (200-300 mesh, H+ form, manufactured by Mitsubishi Chemical Industries Limited)
  4. washwashed with water
  5. washeluted with 3% ammonium hydroxide solution
  6. washThe fraction eluted from 3% ammonium hydroxide solution
  7. customwas evaporated to dryness

出典と根拠

ORDレコード
ord-d3d532daac044f4e9c52d208f1fc7b58
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04069318

反応ノート

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