1,2-Dichloroethane → HCID 178452378、化合物

HRID 1185541ノート

反応式

HRID 1185541 の反応式
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([CH3:13])=[C:9]([CH3:12])[CH:10]=2)[N:5]=[C:4]([C:14]([OH:16])=O)[CH:3]=1.[CH2:17]([O:21][C:22]([N:24]1[CH2:29][CH2:28][N:27]([C:30](=[O:33])[CH2:31][NH2:32])[CH2:26][CH2:25]1)=[O:23])[CH2:18][CH2:19][CH3:20].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C.O>[CH2:17]([O:21][C:22]([N:24]1[CH2:25][CH2:26][N:27]([C:30](=[O:33])[CH2:31][NH:32][C:14]([C:4]2[CH:3]=[C:2]([OH:1])[C:11]3[C:6](=[CH:7][C:8]([CH3:13])=[C:9]([CH3:12])[CH:10]=3)[N:5]=2)=[O:16])[CH2:28][CH2:29]1)=[O:23])[CH2:18][CH2:19][CH3:20]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 667130634-(2-Amino-acetyl)-piperazine-1-carboxylic acid butyl esterHCID 178422310HCID 178422310、化合物

生成物 1

HCID 178452378HCID 178452378、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 100 mg of 4-Hydroxy-6,7-dimethyl-quinoline-2-carboxylic acid and 164 mg of 4-(2-Amino-acetyl)-piperazine-1-carboxylic acid butyl ester in 1 ml of DMF, 70 mg of HOBT and 88 mg of EDC was added and the reaction mixture was stirred for 4 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 and the isolated crude product was pure enough for the next reaction step. Yield: 250 mg.

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 isolated crude product
  5. customwas pure enough for the next reaction step

出典と根拠

ORDレコード
ord-b9820dab69e64761a41dc968d6d6b3a0
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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