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

HRID 1678455
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반응식

HRID 1678455 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-962cae0f652648a7a3b2a7d6b16275ea
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008303B2

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