1,2-Dichloroethane → (E)-3-(dimethylamino)-5-(4-hydroxy-3,5-dimethylstyryl)-N-propylbenzamide

HRID 2368879ノート

反応式

HRID 2368879 の反応式
[CH3:1][N:2]([CH3:26])[C:3]1[CH:4]=[C:5]([CH:9]=[C:10](/[CH:12]=[CH:13]/[C:14]2[CH:19]=[C:18]([CH3:20])[C:17]([O:21]COC)=[C:16]([CH3:25])[CH:15]=2)[CH:11]=1)[C:6](O)=[O:7].C(Cl)CCl.C1C=[N:35][C:34]2N(O)N=N[C:33]=2[CH:32]=1.C(N)CC>CN(C1C=CN=CC=1)C.CN(C=O)C.CCOC(C)=O>[CH3:26][N:2]([CH3:1])[C:3]1[CH:4]=[C:5]([CH:9]=[C:10](/[CH:12]=[CH:13]/[C:14]2[CH:15]=[C:16]([CH3:25])[C:17]([OH:21])=[C:18]([CH3:20])[CH:19]=2)[CH:11]=1)[C:6]([NH:35][CH2:34][CH2:33][CH3:32])=[O:7]

参加物

8

反応物 4

HCID 111,2-DichloroethaneHCID 7852PropylamineHCID 181649HOAtHCID 67262210(E)-3-(dimethylamino)-5-(4-(methoxymethoxy)-3,5-dimethylstyryl)benzoic acid

生成物 1

HCID 67256446(E)-3-(dimethylamino)-5-(4-hydroxy-3,5-dimethylstyryl)-N-propylbenzamide

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 5 (80 mg, 0.225 mmol), EDC (88 mg, 0.45 mmol), HOAT (61.2 mg, 0.45 mmol), and DMAP (5.5 mg, 0.045 mmol) in 2 mL of DMF was added propylamine (37.8 □L, 0.45 mmol) at room temperature. The reaction mixture was stirred overnight (about 18 hours) and diluted with EtOAc. The solution was washed with brine and dried with Na2SO4. The solution was filtered and concentrated.

後処理

  1. washThe solution was washed with brine
  2. dry with materialdried with Na2SO4
  3. filtrationThe solution was filtered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-2202c4e260094d93a5bcdcb72b704ca9
出典データセット
uspto-grants-2014_04
特許番号
US08703815B2

反応ノート

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