HCID 86602935, 화합물 → HCID 59699536, 화합물

HRID 1868181노트

반응식

HRID 1868181 반응식
C([O:8][C@@H:9]1[C@@H:40]([O:41]CC2C=CC=CC=2)[C@H:39]([O:49][C@H:50]2[O:79][C@H:78]([CH3:80])[C@@H:69]([O:70]CC3C=CC=CC=3)[C@H:60]([O:61]CC3C=CC=CC=3)[C@H:51]2[O:52]CC2C=CC=CC=2)[C@@H:38]([CH2:81][O:82]CC2C=CC=CC=2)[O:37][C@@H:10]1[O:11][C@H:12]1[C@H:16]([F:17])[CH2:15][N:14](C(OCC2C=CC=CC=2)=O)[C@@H:13]1[CH2:28][O:29]CC1C=CC=CC=1)C1C=CC=CC=1>CO.Cl.[OH-].[Pd+2].[OH-].[C]>[C@H:50]1([O:49][C@@H:39]2[C@@H:38]([CH2:81][OH:82])[O:37][C@H:10]([O:11][C@H:12]3[C@H:16]([F:17])[CH2:15][NH:14][C@@H:13]3[CH2:28][OH:29])[C@H:9]([OH:8])[C@H:40]2[OH:41])[O:79][C@H:78]([CH3:80])[C@@H:69]([OH:70])[C@H:60]([OH:61])[C@H:51]1[OH:52]

참가 물질

4

반응물 1

HCID 86602935HCID 86602935, 화합물

생성물 1

HCID 59699536HCID 59699536, 화합물수율 65%

시약·촉매·용매 2

HCID 178502593HCID 178502593, 화합물촉매HCID 21893726Hydrochloride methanol용매

실험 절차

The compound (109 mg, 90.2 μmol) synthesized in Example 9 (9d) was dissolved in 1% hydrochloric acid methanol solution (5 mL) and 20% palladium hydroxide-carbon (55 mg) was added thereto, followed by stirring of the mixture under a hydrogen atmosphere for 1 hour. After the catalyst was removed by celite filtration, 28% ammonia water (0.2 mL) was added thereto and the mixture was stirred for 10 minutes. After the solvent was distilled off under reduced pressure and it was passed through ion exchange resin (Dowex 50w×8) column with water (30 mL), 1% ammonia water (30 mL) was flowed through. The ammonia water containing the desired compound was concentrated under reduced pressure and the residue was purified using silica gel flash column chromatography (ethyl acetate:methanol:water, 5:2:1-1:1:1, V/V) to obtain the desired title compound (26 mg, 65%) as a colorless solid.

후처리

  1. customAfter the catalyst was removed by celite filtration, 28% ammonia water (0.2 mL)
  2. additionwas added
  3. stirringthe mixture was stirred for 10 minutes
  4. distillationAfter the solvent was distilled off under reduced pressure and it
  5. concentrationThe ammonia water containing the desired compound was concentrated under reduced pressure
  6. customthe residue was purified

출처 및 근거

ORD 기록
ord-35b403357f204e6cb9fc88ccce163086
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07632930B2

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