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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 10627240, 화합물 → Hexanamide, 3,6-diamino-N-(2-aminoethyl)-, (R)-

HRID 1457951
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HRID 1457951 반응식
C(OC([NH:11][C@H:12]([CH2:30][CH2:31][CH2:32][NH:33]C(OCC1C=CC=CC=1)=O)[CH2:13][C:14]([NH:16][CH2:17][CH2:18][NH:19]C(OCC1C=CC=CC=1)=O)=[O:15])=O)C1C=CC=CC=1.[H][H]>CO.O.[C].[Pd]>[NH2:11][C@H:12]([CH2:30][CH2:31][CH2:32][NH2:33])[CH2:13][C:14]([NH:16][CH2:17][CH2:18][NH2:19])=[O:15]
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참가 물질

6

반응물 2

HCID 10627240HCID 10627240, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 3001582Hexanamide, 3,6-diamino-N-(2-aminoethyl)-, (R)-수율 98.9%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매HCID 962Water
용매
2회

실험 절차

In 180 ml of methanol were suspended 1.41 g (2.39 mmol) of (R)-3,6-bis(benzyloxycarbonylamino)-N-(2-benzyloxycarbonylaminoethyl)hexanamide. To the resulting suspension was added a suspension of 718 mg of 10% palladium-carbon in 20 ml of water. After stirring, hydrogen gas was passed through the resulting mixture at room temperature for 3 hours to effect the reaction. The palladium-corbon was filtered off from the reaction mixture obtained, and the filtrate was concentrated to dryness. The residue obtained was dissolved in 15 ml of water and then subjected to a chromatography on a column of "Amberlite CG-50" (trade name, NH4+ -form, 50 ml). After the column was washed with 200 ml of water, the column was eluted with aqueous ammonia at concentrations gradiently varying from 0.5% to 4.0% (0.5%-increased steps; 200 ml at each concentration). Fractions of the eluate as eluted with 2.5% to 3.5% aqueous ammonia were combined together and concentrated to dryness, to afford 445 mg of (R)-3,6-diamino-N-(2-aminoethyl)hexanamide as a colorless paste.

후처리

  1. additionTo the resulting suspension was added
  2. customthe reaction
  3. filtrationThe palladium-corbon was filtered off from the reaction mixture
  4. customobtained
  5. concentrationthe filtrate was concentrated to dryness
  6. customThe residue obtained
  7. washAfter the column was washed with 200 ml of water
  8. washthe column was eluted with aqueous ammonia at concentrations
  9. temperatureincreased steps
  10. concentration200 ml at each concentration)
  11. washFractions of the eluate as eluted with 2.5% to 3.5% aqueous ammonia
  12. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-4eaf32e6ecdf45e6b5aad3ff5772ceb6
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849797

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