1,2-Dichloroethane → HCID 178452376、化合物

HRID 1185593ノート

反応式

HRID 1185593 の反応式
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]([OH:14])=O)[CH:3]=1.[CH2:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][N:25]([C:28](=[O:31])[CH2:29][NH2:30])[CH2:24][CH2:23]1)=[O:21])[CH2:16][CH2:17][CH3:18].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C.O>[CH2:15]([O:19][C:20]([N:22]1[CH2:23][CH2:24][N:25]([C:28](=[O:31])[CH2:29][NH:30][C:12]([C:4]2[CH:3]=[C:2]([OH:1])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[N:5]=2)=[O:14])[CH2:26][CH2:27]1)=[O:21])[CH2:16][CH2:17][CH3:18]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 667130634-(2-Amino-acetyl)-piperazine-1-carboxylic acid butyl esterHCID 178418933HCID 178418933、化合物

生成物 1

HCID 178452376HCID 178452376、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 9.5 g of 4-Hydroxy-quinoline-2-carboxylic acid and 12.2 g of 4-(2-Amino-acetyl)-piperazine-1-carboxylic acid butyl ester in 110 ml of DMF, 7.7 g of HOBT and 9.6 g of EDC was added and the reaction mixture was stirred for 16 h at RT. Then, the reaction mixture was diluted with water and extracted with DCM. The combined organic phases were dried over MgSO4 and the solvents were removed under reduced pressure. The isolated crude product was used in the next reaction step. Yield: 23 g.

後処理

  1. extractionextracted with DCM
  2. dry with materialThe combined organic phases were dried over MgSO4
  3. customthe solvents were removed under reduced pressure
  4. customThe isolated crude product
  5. customwas used in the next reaction step

出典と根拠

ORDレコード
ord-1ee5a3baee454be6a10eccbbf6eade0e
出典データセット
uspto-grants-2014_03
特許番号
US08669266B2

反応ノート

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