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Oxalic Acid → 4'-(2-Phenoxy-ethylsulfanylmethyl)-biphenyl-3-carboxylic acid(3-dimethylamino-propyl)-amide oxalate

HRID 719679
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반응식

HRID 719679 반응식
[CH3:1][N:2]([CH3:32])[CH2:3][CH2:4][CH2:5][NH:6][C:7]([C:9]1[CH:10]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([CH2:21][S:22][CH2:23][CH2:24][O:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)=[CH:17][CH:16]=2)[CH:12]=[CH:13][CH:14]=1)=[O:8].[C:33]([OH:38])(=[O:37])[C:34]([OH:36])=[O:35].CCOCC>CC(C)=O>[C:33]([OH:38])(=[O:37])[C:34]([OH:36])=[O:35].[CH3:32][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][NH:6][C:7]([C:9]1[CH:10]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([CH2:21][S:22][CH2:23][CH2:24][O:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)=[CH:17][CH:16]=2)[CH:12]=[CH:13][CH:14]=1)=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 971Oxalic AcidHCID 3283Diethyl EtherHCID 103471824'-(2-Phenoxy-ethylsulfanylmethyl)-biphenyl-3-carboxylic acid(3-dimethylamino-propyl)-amide

생성물 1

HCID 103471814'-(2-Phenoxy-ethylsulfanylmethyl)-biphenyl-3-carboxylic acid(3-dimethylamino-propyl)-amide oxalate수율 38.5%

시약·촉매·용매 1

HCID 180Acetone
용매
2회

실험 절차

Dissolved 4′-(2-phenoxy-ethylsulfanylmethyl)-biphenyl-3-carboxylic acid(3-dimethylamino-propyl)-amide (0.48 g, 1.07 mmol, 1 eq.) in acetone (10 mL) and treated the solution dropwise with oxalic acid(0.12 g, 1.28 mmol, 1.2 eq.) in acetone (5 mL). Added Et2O until cloudy and then placed in the freezer to induce crystallization. The resulting white solid was collected by filtration and washed with Et2O to give 4′-(2-phenoxy-ethylsulfanylmethyl)-biphenyl-3-carboxylic acid(3-dimethylamino-propyl)-amide oxalate (0.2217 g).

후처리

  1. customcrystallization
  2. filtrationThe resulting white solid was collected by filtration
  3. washwashed with Et2O

출처 및 근거

ORD 기록
ord-a3b96aeb213a43cc9e01ca5a60ccbd40
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07132456B2

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