HCID 178477443、化合物 → HCID 178477444、化合物

HRID 1834876ノート

反応式

HRID 1834876 の反応式
[N:1]#[N:2].C([O:7][C:8](=[O:44])[CH2:9][N:10]([C:16](=[O:43])[C@H:17]([CH2:36][CH2:37][CH2:38][NH:39][C:40](=[NH:42])[NH2:41])[NH:18][S:19]([C:22]1[CH:31]=[CH:30][C:29]2[C:24](=[CH:25][C:26]([O:34][CH3:35])=[C:27]([O:32][CH3:33])[CH:28]=2)[CH:23]=1)(=[O:21])=[O:20])[CH2:11][CH2:12][S:13][CH2:14][CH3:15])(C)(C)C>FC(F)(F)C(O)=O>[N:1]#[N:2].[CH3:33][O:32][C:27]1[CH:28]=[C:29]2[C:24](=[CH:25][C:26]=1[O:34][CH3:35])[CH:23]=[C:22]([S:19]([NH:18][C@H:17]([C:16]([N:10]([CH2:11][CH2:12][S:13][CH2:14][CH3:15])[CH2:9][C:8]([OH:44])=[O:7])=[O:43])[CH2:36][CH2:37][CH2:38][NH:39][C:40](=[NH:41])[NH2:42])(=[O:21])=[O:20])[CH:31]=[CH:30]2

参加物

3

反応物 1

HCID 178477443HCID 178477443、化合物

生成物 1

HCID 178477444HCID 178477444、化合物収率 26.3%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 5.0 g of N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl-N-(2-ethylthioethyl)glycine tert-butyl ester in 10 ml of trifluoroacetic acid 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 ethanol-H2O-NH4OH (5:4:1). The main fraction eluted from the ethanol-H2O-NH4OH solution was evaporated to dryness to give a crystalline material. This was recrystallized from water to give 1.2 g of N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl-N-(2-ethylthioethyl) glycine, M.P. 171°-2° C.

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 ethanol-H2O-NH4OH (5:4:1)
  6. washThe main fraction eluted from the ethanol-H2O-NH4OH solution
  7. customwas evaporated to dryness
  8. customto give a crystalline material
  9. customThis was recrystallized from water

出典と根拠

ORDレコード
ord-06fa088ec27b4794ad40696b67d383b6
出典データセット
uspto-grants-1978_01
特許番号
US04071621

反応ノート

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