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Oxalyl chloride → HCID 178491050、化合物

HRID 1946245
ノート
印刷プレビュー

反応式

HRID 1946245 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 212753225-Cyano-2-methoxybenzoyl chlorideHCID 219425685-Cyano-2-methoxybenzoic acidHCID 178508054HCID 178508054、化合物

生成物 1

HCID 178491050HCID 178491050、化合物収率 11.9%

試薬・触媒・溶媒

3
HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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]

出典と根拠

ORDレコード
ord-85a248a922774a20bb47ae4240c2ed0b
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399442B2

反応ノート

読み込み中…

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