1,2-Dichloroethane → HCID 178473381、化合物

HRID 1908623ノート

反応式

HRID 1908623 の反応式
[OH:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([C:13]([OH:15])=O)[CH:3]=1.[CH2:16]([O:18][C:19]([N:21]1[CH2:26][CH2:25][N:24]([C:27](=[O:40])[C@@H:28]([NH2:39])[CH2:29][CH2:30][CH2:31][C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:23][CH2:22]1)=[O:20])[CH3:17].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C.O>[CH2:16]([O:18][C:19]([N:21]1[CH2:22][CH2:23][N:24]([C:27](=[O:40])[C@@H:28]([NH:39][C:13]([C:4]2[CH:3]=[C:2]([OH:1])[N:6]([C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=3)[N:5]=2)=[O:15])[CH2:29][CH2:30][CH2:31][C:32]([O:34][C:35]([CH3:37])([CH3:36])[CH3:38])=[O:33])[CH2:25][CH2:26]1)=[O:20])[CH3:17]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 669199764-((S)-2-Amino-5-tert-butoxycarbonyl-pentanoyl)-piperazine-1-carboxylic acid ethyl esterHCID 178524628HCID 178524628、化合物

生成物 1

HCID 178473381HCID 178473381、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 171 mg of 5-Hydroxy-1-phenyl-1H-pyrazole-3-carboxylic acid and 300 mg of 4-((S)-2-Amino-5-tert-butoxycarbonyl-pentanoyl)-piperazine-1-carboxylic acid ethyl ester in 3 ml of DMF, 128 mg of HOBT and 160 mg of EDC was added and the reaction mixture was stirred for 5 h at RT. Then, the reaction mixture was diluted with water and filtered through a Chem Elut® cartridge by eluting with ethyl acetate. The solvents were removed under reduced pressure. The solid product was triturated with DCM and the precipitate was dried under reduced pressure. The crude product was used in the subsequent reaction.

後処理

  1. filtrationfiltered through a Chem Elut® cartridge
  2. washby eluting with ethyl acetate
  3. customThe solvents were removed under reduced pressure
  4. customThe solid product was triturated with DCM
  5. customthe precipitate was dried under reduced pressure
  6. customThe crude product was used in the subsequent reaction

出典と根拠

ORDレコード
ord-2054c1a39ada407d981ca260ecbdea4d
出典データセット
uspto-grants-2013_12
特許番号
US08598179B2

反応ノート

読み込み中…