Morpholine → 4'-(4-Morpholinylcarbonyl)[1,1'-biphenyl]-4-ol

HRID 494779노트

반응식

HRID 494779 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]([OH:16])=O)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1.C(N(CC)CC)C.Cl.CN(C)CCCN=C=NCC>ClCCl>[N:17]1([C:14]([C:11]2[CH:10]=[CH:9][C:8]([C:5]3[CH:4]=[CH:3][C:2]([OH:1])=[CH:7][CH:6]=3)=[CH:13][CH:12]=2)=[O:16])[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1

참가 물질

6

반응물 4

HCID 8083MorpholineHCID 8471TriethylamineHCID 3015564'-Hydroxy-4-biphenylcarboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 222746894'-(4-Morpholinylcarbonyl)[1,1'-biphenyl]-4-ol수율 83.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-hydroxy-biphenyl-4′-carboxylic acid (5.35 g, 25.0 mmol), morpholine (2.39 g, 27.5 mmol) and triethylamine (3.5 mL, 25 mmol) in dichloromethane (100 mL) was added 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride. The mixture was stirred for 16 hours, diluted with aqueous NaH2PO4 and filtered. The solid was washed with 1:2 diethyl ether/water (100 mL) then with water (400 mL). The solid was dried in vacuo to give the titled compound (5.89 g, 83%). MS (DCI) m/z 284 (M+H)+;

후처리

  1. filtrationfiltered
  2. washThe solid was washed with 1:2 diethyl ether/water (100 mL)
  3. customThe solid was dried in vacuo

출처 및 근거

ORD 기록
ord-3c4e521ae07245b9b70a018e38637a0e
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538138B2

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