4-Piperidineethanol → HCID 13336380, 화합물

HRID 986288노트

반응식

HRID 986288 반응식
[C:1]1([C:7]2[N:16]=[C:15]([C:17]([O:19]CC)=O)[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH:22]1[CH2:27][CH2:26][CH:25]([CH2:28][CH2:29][OH:30])[CH2:24][CH2:23]1>O>[C:1]1([C:7]2[N:16]=[C:15]([C:17]([N:22]3[CH2:27][CH2:26][CH:25]([CH2:28][CH2:29][OH:30])[CH2:24][CH2:23]3)=[O:19])[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 739534-PiperidineethanolHCID 20158356HCID 20158356, 화합물

생성물 1

HCID 13336380HCID 13336380, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Ethyl 2-phenylquinazoline-4-carboxylate (1.7 g) and piperidine-4-ethanol (8 g) are heated at 150° C. for 4 hours. After cooling, water is added and the mixture is extracted with ethyl acetate. The organic phase is dried over magnesium sulphate and evaporated to dryness under reduced pressure. The residue is chromatographed on silica gel with ethyl acetate as the eluant, and the product recovered is recrystallized from isopropyl ether. This gives 1-[(2-phenylquinazolin-4-yl)-carbonyl]-piperidine-4-ethanol (0.5 g), melting at 146° C.

후처리

  1. temperatureAfter cooling
  2. extractionthe mixture is extracted with ethyl acetate
  3. dry with materialThe organic phase is dried over magnesium sulphate
  4. customevaporated to dryness under reduced pressure
  5. customThe residue is chromatographed on silica gel with ethyl acetate as the eluant
  6. customthe product recovered
  7. customis recrystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-670b5c065a944f6995ddfc6a0c7e14ac
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04711890

반응 노트

불러오는 중…