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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 59596400, 화합물 → HCID 59596404, 화합물

HRID 2264584
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HRID 2264584 반응식
[F:1][C:2]([F:41])([F:40])[C:3]1[CH:4]=[C:5]([NH:17][C:18]([N:20]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]3[CH:27]=[C:28]([O:31][C:32]4[CH:37]=[C:36](Cl)[N:35]=[C:34]([NH2:39])[N:33]=4)[CH:29]=[CH:30][C:21]2=3)=[O:19])[CH:6]=[CH:7][C:8]=1[CH2:9][N:10]1[CH2:15][CH2:14][N:13]([CH3:16])[CH2:12][CH2:11]1>CO.[Pd]>[F:41][C:2]([F:1])([F:40])[C:3]1[CH:4]=[C:5]([NH:17][C:18]([N:20]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]3[CH:27]=[C:28]([O:31][C:32]4[CH:37]=[CH:36][N:35]=[C:34]([NH2:39])[N:33]=4)[CH:29]=[CH:30][C:21]2=3)=[O:19])[CH:6]=[CH:7][C:8]=1[CH2:9][N:10]1[CH2:15][CH2:14][N:13]([CH3:16])[CH2:12][CH2:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 59596400HCID 59596400, 화합물

생성물 1

HCID 59596404HCID 59596404, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

250 mg (0.42 mMol) of 7-(2-amino-6-chloro-pyrimidin-4-yloxy)-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid [3-trifluoromethyl-4-(4-methylpiperazin-1-ylmethyl)-phenyl]-amide in 35 ml methanol are hydrogenated in the presence of 160 mg Pd/C (10%; Engelhard 4505). The catalyst is filtered off, the filtrate diluted with EtOAc and sat. Na2CO3/H2O 1:1 and the separated aqueous layer extracted twice with water. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Reversed phase MPLC (Gilson system) gives the title compound: MS: [M+1]+=556; HPLC: AtRet=9.0.

후처리

  1. filtrationThe catalyst is filtered off
  2. additionthe filtrate diluted with EtOAc and sat. Na2CO3/H2O 1:1
  3. extractionthe separated aqueous layer extracted twice with water
  4. washThe organic layers are washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b8c7a00f185c4cd382a0e639176eada3
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07855215B2

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