Dichloromethane → HCID 67235119、化合物

HRID 1505318ノート

反応式

HRID 1505318 の反応式
[CH3:1][C@@H:2]([NH:22]C(=O)OC(C)(C)C)[C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]([O:20][CH3:21])[CH:14]=2)=[CH:8][CH:7]=1)=[O:4].ClCCl>>[CH3:19][C:16]1[CH:17]=[CH:18][C:13]([O:12][C:9]2[CH:10]=[CH:11][C:6]([NH:5][C:3](=[O:4])[C@@H:2]([CH3:1])[NH2:22])=[CH:7][CH:8]=2)=[CH:14][C:15]=1[O:20][CH3:21]

参加物

3

反応物 2

HCID 6344DichloromethaneHCID 68322429HCID 68322429、化合物2 回

生成物 1

HCID 67235119HCID 67235119、化合物収率 97.3%

実験手順

To a solution of 1,1-dimethylethyl {(1R)-1-methyl-2-[(4-{[4-methyl-3-(methyloxy)phenyl]oxy}phenyl)amino]-2-oxoethyl}carbamate (Intermediate 21, 300 mg) in dry dichloromethane (7.5 mL) TFA (2.5 mL, 32.4 mmol) was slowly added and the reaction mixture was stirred for 1.5 hours at room temperature. The solvent and the excess of TFA were evaporated and the residue was purified by SCX cartridge (10 g) to afford the title compound as an orange oil (219 mg).

後処理

  1. customThe solvent and the excess of TFA were evaporated
  2. customthe residue was purified by SCX cartridge (10 g)

出典と根拠

ORDレコード
ord-5fc28f03edb34c5c944f156534275047
出典データセット
uspto-grants-2015_12
特許番号
US09216967B2

反応ノート

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