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Hydrazine hydrate (1:1) → HCID 178446045, 화합물

HRID 1279184
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HRID 1279184 반응식
[NH:1]([C:23]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:24])[C@H:2]([C:7]([NH:9][C@H:10]([C:18](OCC)=[O:19])[CH2:11][CH2:12][CH2:13][NH:14][C:15](=[NH:17])[NH2:16])=[O:8])[CH2:3][CH:4]([CH3:6])[CH3:5].[NH2:33][NH2:34].O>CO>[NH:1]([C:23]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:24])[C@H:2]([C:7]([NH:9][C@H:10]([C:18]([NH:33][NH2:34])=[O:19])[CH2:11][CH2:12][CH2:13][NH:14][C:15](=[NH:17])[NH2:16])=[O:8])[CH2:3][CH:4]([CH3:6])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 178472555HCID 178472555, 화합물

생성물 1

HCID 178446045HCID 178446045, 화합물수율 74.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Z-Leu-Arg-OEt was dissolved in 500 mL of methanol. NH2NH2.H2O 150 mL was added with ice cooling to the solution, then the mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated under reduced pressure, 500 mL of water was added to the obtained residue, then the product was extracted 5 times with 1000 mL of n-butanol. The extract was washed 4 times with 500 mL of water, then concentrated under reduced pressure. The resulting residue was solidified by treatment with ether, then it was dried. Thus, 209.7 g of Z-Leu-Arg-NHNH2 (74.1% yield) was obtained.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, 500 mL of water
  2. additionwas added to the obtained residue
  3. extractionthe product was extracted 5 times with 1000 mL of n-butanol
  4. washThe extract was washed 4 times with 500 mL of water
  5. concentrationconcentrated under reduced pressure
  6. customit was dried

출처 및 근거

ORD 기록
ord-e6ab8379edf84513b4f5bc286700bbc0
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06448031B1

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