Triethylamine → HCID 178496913、化合物

HRID 2419031ノート

反応式

HRID 2419031 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 178496913HCID 178496913、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-49b5163e1104467baab56ce5102838f7
出典データセット
uspto-grants-1978_08
特許番号
US04104392

反応ノート

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