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Oxalyl chloride → HCID 178491050, 화합물

HRID 1639607
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HRID 1639607 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:12][CH3:13])=[C:7]([CH:11]=1)[C:8]([OH:10])=O)#[N:2].C(Cl)(=O)C(Cl)=O.[N:20]1([CH2:26][C:27]2[CH:41]=[CH:40][C:30]3[NH:31][C:32]([C:34]4[C:38]([NH2:39])=[CH:37][NH:36][N:35]=4)=[N:33][C:29]=3[CH:28]=2)[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1.C(C1C=CC(OC)=C(C=1)C(Cl)=O)#N.C(N(C(C)C)CC)(C)C>C(Cl)Cl.CN(C=O)C.C1COCC1>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:12][CH3:13])=[C:7]([CH:11]=1)[C:8]([NH:39][C:38]1[C:34]([C:32]2[NH:31][C:30]3[CH:40]=[CH:41][C:27]([CH2:26][N:20]4[CH2:21][CH2:22][O:23][CH2:24][CH2:25]4)=[CH:28][C:29]=3[N:33]=2)=[N:35][NH:36][CH:37]=1)=[O:10])#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 212753225-Cyano-2-methoxybenzoyl chlorideHCID 219425685-Cyano-2-methoxybenzoic acidHCID 178508054HCID 178508054, 화합물

생성물 1

HCID 178491050HCID 178491050, 화합물수율 11.9%

시약·촉매·용매

3
HCID 6228Dimethylformamide촉매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

5-Cyano-2-methoxy-benzoic acid (Example 1F) (40 mg, 0.22 mmol) was dissolved in DCM (5 ml) and oxalyl chloride (34.4 mg, 0.264 mmol) was then added drop wise followed by DMF (1 drop). The reaction mixture was stirred at ambient temperature for 1 hour, reduced in vacuo, then re-evaporated using toluene (×2). A mixture of 3-(5-morpholin-4-ylmethyl-1H-benzimidazol-2-yl)-1H-pyrazol-4-ylamine (100 mg, 0.33 mmol), 5-cyano-2-methoxy-benzoyl chloride and diisopropylethylamine (1.83 μl, 0.9 mmol) in THF (5 ml) was stirred at 0° C. and then allowed to warm to room temperature over 2 hours. The reaction mixture was then concentrated in vacuo. The residue was purified by flash column chromatography SiO2, 5-7% MeOH-DCM] to give 5-cyano-2-methoxy-N-[3-(5-morpholin-4-ylmethyl-1H-benzoimidazol-2-yl)-1H-pyrazol-4-yl]-benzamide (12 mg). (LC/MS Acidic: Rt 2.02 min [M−H]+ 458).

후처리

  1. customre-evaporated
  2. stirringwas stirred at 0° C.
  3. temperatureto warm to room temperature over 2 hours
  4. concentrationThe reaction mixture was then concentrated in vacuo
  5. customThe residue was purified by flash column chromatography SiO2, 5-7% MeOH-DCM]

출처 및 근거

ORD 기록
ord-2402b28fd7044dfa87dcd3fa910facd9
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08110573B2

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