Ethanol → HCID 86625841、化合物

HRID 644140ノート

反応式

HRID 644140 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 86625841HCID 86625841、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c75d0d292c3f4168894bd30163bf0922
出典データセット
uspto-grants-2010_04
特許番号
US07700623B2

反応ノート

読み込み中…