HCID 178477443, 화합물 → HCID 178477444, 화합물

HRID 1834876노트

반응식

HRID 1834876 반응식
[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

참가 물질

3

반응물 1

HCID 178477443HCID 178477443, 화합물

생성물 1

HCID 178477444HCID 178477444, 화합물수율 26.3%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-06fa088ec27b4794ad40696b67d383b6
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04071621

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