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HCID 10461505, 화합물 → HCID 54514397, 화합물

HRID 1462373
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HRID 1462373 반응식
[C:1]([C:4]1[CH:5]=[C:6]([CH:43]=[CH:44][C:45]=1[OH:46])[O:7][CH2:8][CH2:9][N:10](CC1C=CC=CC=1)[CH2:11][CH:12]([C:14]1[CH:19]=[C:18]([O:20]CC2C=CC=CC=2)[CH:17]=[C:16]([O:28]CC2C=CC=CC=2)[CH:15]=1)[OH:13])(=[O:3])[NH2:2].[H][H]>CO.[Pd]>[C:1]([C:4]1[CH:5]=[C:6]([CH:43]=[CH:44][C:45]=1[OH:46])[O:7][CH2:8][CH2:9][NH:10][CH2:11][CH:12]([OH:13])[C:14]1[CH:19]=[C:18]([OH:20])[CH:17]=[C:16]([OH:28])[CH:15]=1)(=[O:3])[NH2:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10461505HCID 10461505, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 54514397HCID 54514397, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A solution of 31 g of crude N-[2-(3-carbamoyl-4-hydroxyphenoxy)-ethyl]-N-[2-(3,5-dibenzyloxyphenyl)-2-hydroxy-ethyl]-benzylamine in 300 ml of methanol is hydrogenated under normal conditions over 6 g of palladium-on-charcoal catalyst (5%) until 3 mol equivalents of hydrogen have been taken up. The catalyst is filtered off, the filtrate is evaporated and the residue is dissolved in 200 ml of isopropanol. Filtering through silica gel and evaporating the filtrate yields α-[N-[2-(3-carbamoyl-4-hydroxyphenoxy)-ethyl]aminomethyl]-3,5-dihydroxy-benzyl alcohol in the form of a brownish foam. After recrystallisation from ethylacetate/methanol the compound is obtained in pure state with a melting point of 203°-205°, and contains 1/4 mol of crystal-water. The compound is characterised by the following signals in the proton nuclear magnetic resonance spectrum in hexadeuterodimethylsulfoxide as the solvent:

후처리

  1. filtrationThe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. dissolutionthe residue is dissolved in 200 ml of isopropanol
  4. filtrationFiltering through silica gel
  5. customevaporating the filtrate

출처 및 근거

ORD 기록
ord-1e849d3b9ea14ee0b59637a364f33d88
출처 데이터셋
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04460580

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