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4-Methylmorpholine → 2'-Methyl-5'-(4-morpholin-4-yl-benzoylamino)-biphenyl-4-carboxylic acid ethyl ester

HRID 1678455
ノート
印刷プレビュー

反応式

HRID 1678455 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[C:16]([NH2:18])[CH:15]=[CH:14][C:13]=2[CH3:19])=[CH:8][CH:7]=1)=[O:5])[CH3:2].[N:20]1([C:26]2[CH:34]=[CH:33][C:29]([C:30](O)=[O:31])=[CH:28][CH:27]=2)[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1.CN1CCOCC1.ON1C2C=CC=CC=2N=N1.Cl.CN(CCCN=C=N)C>CN(C=O)C>[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[CH:8][C:9]([C:12]2[CH:17]=[C:16]([NH:18][C:30](=[O:31])[C:29]3[CH:28]=[CH:27][C:26]([N:20]4[CH2:25][CH2:24][O:23][CH2:22][CH2:21]4)=[CH:34][CH:33]=3)[CH:15]=[CH:14][C:13]=2[CH3:19])=[CH:10][CH:11]=1)=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 3452784-(Morpholin-4-yl)benzoic acidHCID 21899179Dimethylaminopropyl carbodiimide hydrochlorideHCID 598223355'-Amino-2'-methyl-biphenyl-4-carboxylic acid ethyl ester

生成物 1

HCID 59822331
2'-Methyl-5'-(4-morpholin-4-yl-benzoylamino)-biphenyl-4-carboxylic acid ethyl ester
収率 88.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5′-Amino-2′-methyl-biphenyl-4-carboxylic acid ethyl ester (2.15 g), 4-morpholin-4-yl benzoic acid (1.27 g), N-methylmorpholine (2.05 ml), 1-hydroxybenzotriazole (826 mg) and 1-ethyl-3-(3-(dimethylaminopropyl)carbodiimide hydrochloride (1.17 g) in dry DMF (30 ml) was stirred at 20 C for 18 h. Then the DMF was evaporated and the residue partitioned between water and dichloromethane. The dried extracts were evaporated and the residue purified on silica gel. Elution with 1-2% methanol in dichloromethane gave a colourless solid (2.4 g)

後処理

  1. customThen the DMF was evaporated
  2. customthe residue partitioned between water and dichloromethane
  3. customThe dried extracts were evaporated
  4. customthe residue purified on silica gel
  5. washElution with 1-2% methanol in dichloromethane

出典と根拠

ORDレコード
ord-962cae0f652648a7a3b2a7d6b16275ea
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08008303B2

反応ノート

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