Ethanol → HCID 86625841, 화합물

HRID 644140노트

반응식

HRID 644140 반응식
C(O)C.C(O[C:7](=[NH:37])[C:8]1[CH:36]=[CH:35][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH:16]2[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][CH2:24][O:25][C:26]3[CH:34]=[CH:33][C:29]([C:30](=[NH:32])[O-:31])=[CH:28][CH:27]=3)[CH2:18][CH2:17]2)=[CH:10][CH:9]=1)C.Cl.[F:39][C:40]([F:45])([F:44])[CH2:41][O:42][NH2:43].C(N(CC)CC)C>O.C(Cl)(Cl)Cl>[NH2:37][C:7](=[N:43][O:42][CH2:41][C:40]([F:45])([F:44])[F:39])[C:8]1[CH:9]=[CH:10][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH:16]2[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][CH2:24][O:25][C:26]3[CH:34]=[CH:33][C:29]([C:30]([NH2:32])=[O:31])=[CH:28][CH:27]=3)[CH2:18][CH2:17]2)=[CH:35][CH:36]=1

참가 물질

7

반응물 4

HCID 702EthanolHCID 8471TriethylamineHCID 19853822O-(2,2,2-Trifluoroethyl)hydroxylamine hydrochlorideHCID 86625839HCID 86625839, 화합물

생성물 1

HCID 86625841HCID 86625841, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

To an ethanol (6 mL) suspension of 0.20 g of ethyl=4-{3-[4-(3-{4-[ethoxy(imino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzimidate were added 0.61 g of O-(2,2,2-trifluoroethyl)hydroxylamine hydrochloride and 0.84 mL of triethylamine at room temperature, which was then stirred at the same temperature for one week. Chloroform and water were added to the reaction solution. The organic layer was separated, washed with a saturated sodium chloride aqueous solution, and then dried with anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. The resultant residue was purified using silica gel column chromatography (eluent; chloroform:ethanol=30:1), to which hexane was then added, followed by collecting the solid by filtration to provide 0.12 g of 4-{3-[4-(3-{4-[amino(2,2,2-trifluoroethoxyimino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzamide=O-(2,2,2-trifluoroethyl)oxime as white solid form.

후처리

  1. customThe organic layer was separated
  2. washwashed with a saturated sodium chloride aqueous solution
  3. dry with materialdried with anhydrous magnesium sulfate
  4. distillationby distilling off the solvent under reduced pressure
  5. customThe resultant residue was purified
  6. additionto which hexane was then added
  7. customby collecting the solid
  8. filtrationby filtration

출처 및 근거

ORD 기록
ord-c75d0d292c3f4168894bd30163bf0922
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700623B2

반응 노트

불러오는 중…