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Hydrochloric Acid → HCID 178479449, 화합물

HRID 1721004
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HRID 1721004 반응식
[ClH:1].Cl.C([O:7][CH:8](OCCCC)[C@H:9]([CH2:40][CH2:41][CH2:42][NH:43][C:44](=[NH:46])[NH2:45])[NH:10][C:11](=[O:39])[C@H:12]([CH2:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)[NH:13][C:14](=[O:31])[C@H:15]1[CH2:19][CH2:18][C:17](=[O:20])[N:16]1[C:21]([O:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:22])CCC.[OH-].[Na+]>C(#N)C>[ClH:1].[CH2:24]([O:23][C:21]([N:16]1[C:17](=[O:20])[CH2:18][CH2:19][C@@H:15]1[C:14]([NH:13][C@H:12]([C:11]([NH:10][C@H:9]([CH:8]=[O:7])[CH2:40][CH2:41][CH2:42][NH:43][C:44](=[NH:45])[NH2:46])=[O:39])[CH2:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=[O:31])=[O:22])[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178450977HCID 178450977, 화합물

생성물 1

HCID 178479449HCID 178479449, 화합물수율 75%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

After 1N hydrochloric acid aqueous solution (5 ml) was added to a solution of N-benzyloxycarbonyl-D-pyroglutamyl-L-phenylalanyl-L-argininal dibutylacetal hydrochloride (72 mg, 0.10 mmol) in acetonitrile (10 ml), the mixture was reacted at 36° C. for 1.5 hour with stirring. After completion of the reaction, pH of the reaction mixture was adjusted to 4.8 with 1N sodium hydroxide aqueous solution. The solvent was distilled off under reduced pressure and chloroform was added to the residue. Insoluble matters were removed by filtration. After the filtrate was concentrated, the residue was recrystallized from chloroform-hexane to give 44 mg (75%) of N-benzyloxycarbonyl-D-pyroglutamyl-L-phenylalanyl-L-argininal hydrochloride.

후처리

  1. customthe mixture was reacted at 36° C. for 1.5 hour
  2. customAfter completion of the reaction, pH of the reaction mixture
  3. distillationThe solvent was distilled off under reduced pressure and chloroform
  4. additionwas added to the residue
  5. customInsoluble matters were removed by filtration
  6. concentrationAfter the filtrate was concentrated
  7. customthe residue was recrystallized from chloroform-hexane

출처 및 근거

ORD 기록
ord-b08b736cefd84a6fb90c41d133abe44c
출처 데이터셋
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05508385

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