1-Octanol → HCID 67917358, 화합물

HRID 1886332노트

반응식

HRID 1886332 반응식
S(Cl)([Cl:3])=O.[CH2:5]([OH:13])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[CH:14]12[CH2:21][CH2:20][CH:17]([CH2:18][CH2:19]1)[C@@H:16]([C:22](O)=[O:23])[NH:15]2.CCOCC>O.CCOCC>[ClH:3].[CH2:5]([O:13][C:22]([C@@H:16]1[CH:17]2[CH2:20][CH2:21][CH:14]([CH2:19][CH2:18]2)[NH:15]1)=[O:23])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

참가 물질

6

반응물 4

HCID 9571-OctanolHCID 3283Diethyl EtherHCID 24386Thionyl ChlorideHCID 10866570(3S)-2-Azabicyclo[2.2.2]octane-3-carboxylic acid

생성물 1

HCID 67917358HCID 67917358, 화합물수율 81%

시약·촉매·용매 1

HCID 21584184Diethylether water용매

반응 조건

온도
0 °C

실험 절차

9.6 ml of thionyl chloride are added dropwise into a 250 ml round-bottomed flask containing 60 ml of n-octanol cooled to 0° C. After stirring for 10 min at 0° C., 18.6 g of (3S)-2-azabicyclo[2.2.2]octane-3-carboxylic acid (described in Patent FR 2,585,709) are added slowly. The reaction mixture is left stirring overnight at room temperature, then heated for 6 hours at 80° C. and again left overnight at room temperature. After adding 100 ml of anhydrous ether and filtering off the unreacted hydrochloride, the filtrate is condensed and then taken up with a water/ether mixture (50:50). The expected product is obtained after concentration of the aqueous phase and then drying under vacuum.

후처리

  1. waitThe reaction mixture is left
  2. stirringstirring overnight at room temperature
  3. temperatureheated for 6 hours at 80° C. and again left overnight at room temperature
  4. filtrationfiltering off the unreacted hydrochloride
  5. customcondensed

출처 및 근거

ORD 기록
ord-f431ab1817e84c61a7bd674e6802d370
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05151432

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