Triethylamine → HCID 178496913, 화합물

HRID 2419031노트

반응식

HRID 2419031 반응식
Cl.[CH2:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH:4]([C:12]([O:14][CH3:15])=[O:13])[NH:3]1.C(N(CC)CC)C.N#N.Cl.[CH3:26][O:27][C:28]1[CH:29]=[C:30]2[C:35](=[CH:36][C:37]=1[O:38][CH3:39])[CH:34]=[C:33]([S:40]([NH:43][C@H:44]([C:52](Cl)=[O:53])[CH2:45][CH2:46][CH2:47][NH:48][C:49](=[NH:51])[NH2:50])(=[O:42])=[O:41])[CH:32]=[CH:31]2>C(Cl)(Cl)Cl>[CH3:26][O:27][C:28]1[CH:29]=[C:30]2[C:35](=[CH:36][C:37]=1[O:38][CH3:39])[CH:34]=[C:33]([S:40]([NH:43][C@H:44]([C:52]([N:3]1[CH:4]([C:12]([O:14][CH3:15])=[O:13])[CH2:5][C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[CH2:2]1)=[O:53])[CH2:45][CH2:46][CH2:47][NH:48][C:49](=[NH:50])[NH2:51])(=[O:41])=[O:42])[CH:32]=[CH:31]2

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 122480673-Isoquinolinecarboxylic acid, 1,2,3,4-tetrahydro-, methyl ester, hydrochloride (1:1)HCID 178486632HCID 178486632, 화합물

생성물 1

HCID 178496913HCID 178496913, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a stirred solution of 1.8 g of methyl 1,2,3,4-tetrahydroisoquinoline-3-carboxylate hydrochloride and 8 ml of triethylamine in 50 ml of chloroform which was cooled in an ice bath, there was carefully added N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl chloride hydrochloride obtained above. The reaction mixture was allowed to stand overnight at room temperature. The reaction mixture was washed twice with 50 ml of saturated sodium chloride solution and evaporated to dryness. The residue was dissolved in water-ethanol and ajusted to pH 12 with 5N NaOH solution at a temperature below 0° C to precipitate a solid. This was collected by filtration to give 3 g of methyl 2-[N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl]-1,2,3,4-tetrahydroisoquinoline-3-carboxylate.

후처리

  1. customobtained above
  2. washThe reaction mixture was washed twice with 50 ml of saturated sodium chloride solution
  3. customevaporated to dryness
  4. dissolutionThe residue was dissolved in water-ethanol
  5. customajusted to pH 12 with 5N NaOH solution at a temperature below 0° C
  6. customto precipitate a solid
  7. filtrationThis was collected by filtration

출처 및 근거

ORD 기록
ord-49b5163e1104467baab56ce5102838f7
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04104392

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