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Riboflavin → HCID 59547994, 화합물

HRID 1946338
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HRID 1946338 반응식
CC1C=C2N=C3C(=NC(NC3=O)=O)N(C[C@H](O)[C@H](O)[C@H](O)CO)C2=CC=1C.[F:28][C:29]1[CH:56]=[CH:55][CH:54]=[C:53]([F:57])[C:30]=1[C:31]([NH:33][C:34]1[CH:38]=[CH:37][N:36]([CH2:39][C:40]2[CH:45]=[C:44]([N+:46]([O-])=O)[CH:43]=[CH:42][C:41]=2[C:49]([F:52])([F:51])[F:50])[N:35]=1)=[O:32]>[Pd].C(O)C>[NH2:46][C:44]1[CH:43]=[CH:42][C:41]([C:49]([F:51])([F:52])[F:50])=[C:40]([CH2:39][N:36]2[CH:37]=[CH:38][C:34]([NH:33][C:31](=[O:32])[C:30]3[C:29]([F:28])=[CH:56][CH:55]=[CH:54][C:53]=3[F:57])=[N:35]2)[CH:45]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 493570Riboflavin2회HCID 59547920HCID 59547920, 화합물

생성물 1

HCID 59547994HCID 59547994, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매2회HCID 702Ethanol용매

실험 절차

To 10% palladium on activated carbon degussa type E101 NE/W (wet) (440 mg, 4.14 mmol, Aldrich) was added a slight suspension of the 2,6-difluoro-N-(1-{[5-nitro-2-(trifluoromethyl)phenyl]methyl}-1H-pyrazol-3-yl)benzamide (for a preparation see Intermediate 40) (2.0 g, 4.69 mmol) in a solution of ethanol (80 ml) under vacuum. A further amount of 10% palladium on activated carbon degussa type E101 NE/W (wet) (0.2 g) was added after 2 h. The suspension was hydrogenated for a total of 4 h at ambient temperature. The suspension was filtered and the residue washed with ethanol (50 ml). The solvent was removed in vacuo to leave a pale yellow foam (1.79 g); LCMS: (System 4) MH+=397, tRET=2.65 min.

후처리

  1. additionwas added
  2. additionwas added after 2 h
  3. customwas hydrogenated for a total of 4 h at ambient temperature
  4. filtrationThe suspension was filtered
  5. washthe residue washed with ethanol (50 ml)
  6. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-8aedd85d384b482b8a3f56f1fc1f5ab7
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399436B2

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