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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 54110954, 화합물 → HCID 53863065, 화합물

HRID 268178
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반응식

HRID 268178 반응식
C([O:8][C:9]1[CH:10]=[CH:11][C:12]2[N:18]([CH3:19])[C:17](=[O:20])[CH:16]3[CH2:21][CH2:22][CH2:23][N:15]3[CH2:14][C:13]=2[CH:24]=1)C1C=CC=CC=1.[H][H]>[Pd].C(O)C>[OH:8][C:9]1[CH:10]=[CH:11][C:12]2[N:18]([CH3:19])[C:17](=[O:20])[CH:16]3[CH2:21][CH2:22][CH2:23][N:15]3[CH2:14][C:13]=2[CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 54110954HCID 54110954, 화합물HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 53863065HCID 53863065, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A mixture of 6.44 g. of 7-benzyloxy-1,2,3,5,10,11a- hexahydro-10-methyl-11H-pyrrolo[2,1-c] [1,4]benzodiazepin-11- one, 200 ml. of ethanol and 1.0 g. of 10% palladium-on-carbon catalyst is shaken in a Parr hydrogenator under about 3 atmospheric of hydrogen pressure until the theoretical amount of hydrogen is absorbed. The catalyst is filtered off and the mother liquor is concentrated to remove the solvent. The residue is purified by partition chromatography on a diatomaceous earth column using a heptane/methyl cellosolve solvent system to yield pure 1,2,3,5,10,11a-hexahydro-7-hydroxy- 10-methyl-11H-pyrrolo[2,1-c] [1,4]benzodiazepin-11-one.

후처리

  1. additionA mixture of 6.44 g
  2. customis absorbed
  3. filtrationThe catalyst is filtered off
  4. concentrationthe mother liquor is concentrated
  5. customto remove the solvent
  6. customThe residue is purified
  7. customby partition chromatography on a diatomaceous earth column

출처 및 근거

ORD 기록
ord-38834a805c084876aa43b7de5190402d
출처 데이터셋
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03947408

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