Trimethylaluminum → HCID 178489759、化合物

HRID 1911458ノート

反応式

HRID 1911458 の反応式
[CH:1]1([N:4]2[CH2:10][CH2:9][CH2:8][N:7]([C:11]3[CH:21]=[CH:20][C:14]([C:15]([O:17]CC)=O)=[CH:13][CH:12]=3)[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.[CH3:22][O:23][C:24]1[CH:25]=[C:26]([CH2:32][CH2:33][C:34]2[CH:35]=[C:36]([NH2:39])[NH:37][N:38]=2)[CH:27]=[C:28]([O:30][CH3:31])[CH:29]=1.C[Al](C)C.C(Cl)Cl.CCOCC>C1(C)C=CC=CC=1>[CH:1]1([N:4]2[CH2:10][CH2:9][CH2:8][N:7]([C:11]3[CH:12]=[CH:13][C:14]([C:15]([NH:39][C:36]4[NH:37][N:38]=[C:34]([CH2:33][CH2:32][C:26]5[CH:27]=[C:28]([O:30][CH3:31])[CH:29]=[C:24]([O:23][CH3:22])[CH:25]=5)[CH:35]=4)=[O:17])=[CH:20][CH:21]=3)[CH2:6][CH2:5]2)[CH2:2][CH2:3]1

参加物

6

反応物 4

HCID 16682925TrimethylaluminumHCID 21881112Ethyl ether methylene chlorideHCID 66589916Ethyl 4-(4-cyclopropyl-1,4-diazepan-1-yl)benzoateHCID 178489815HCID 178489815、化合物

生成物 1

HCID 178489759HCID 178489759、化合物収率 33.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-(4-cyclopropyl-1,4-diazepan-1-yl)-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]benzamide was prepared using the same procedure as for Example 159, but starting from ethyl 4-(4-cyclopropyl-1,4-diazepan-1-yl)benzoate (0.288 g, 1 mmol, 5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-amine (0.247 g, 1 mmol) and a 2M solution of trimethylaluminium (1.250 mL, 2.50 mmol) in toluene. The crude product was purified by preparative HPLC, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford a gum which solidified on trituration with DCM/Ether to afford the title compound (0.165 g, 33.7%).

後処理

  1. custom4-(4-cyclopropyl-1,4-diazepan-1-yl)-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]benzamide was prepared
  2. customThe crude product was purified by preparative HPLC
  3. additionFractions containing the desired compound
  4. customwere evaporated to dryness
  5. customto afford a gum which

出典と根拠

ORDレコード
ord-713099bb3ca4476bb6bc5dad14f55bba
出典データセット
uspto-grants-2013_12
特許番号
US08604022B2

反応ノート

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