Dimethylformamide → HCID 19800031, 화합물

HRID 1252417노트

반응식

HRID 1252417 반응식
Br[C:2]1[CH:3]=[N:4][C:5]2[C:10]([C:11]=1[NH:12][CH2:13][C:14]1([OH:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)=[CH:9][CH:8]=[CH:7][CH:6]=2.CC(C)([O-])C.[K+].CN(C=O)C>O>[N:12]1[C:11]2[C:10]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:4]=[CH:3][C:2]=2[O:20][C:14]2([CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:13]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 14209243HCID 14209243, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 19800031HCID 19800031, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
130 °C

실험 절차

A mixture of 5.5 g of 3-bromo-N-(1-hydroxycyclohexylmethyl)-4-quinolinamine, 2.2 g of potassium tert-butoxide and 50 ml of DMF was heated at 130° C. for 1 hour and then poured into 250 ml of water. The product was extracted with dichloromethane and ethyl acetate, dried and concentrated, and the residue was purified by HPLC using dichloromethane:MeOH=95:5 as the eluent. The fractions containing the product were combined and concentrated. The residue was taken up in water and stirred for 1 hour, and the solid was filtered and recrystallized from toluene. The yield was 2.6 g, mp 164°-165° C.

후처리

  1. extractionThe product was extracted with dichloromethane and ethyl acetate
  2. customdried
  3. concentrationconcentrated
  4. customthe residue was purified by HPLC
  5. additionThe fractions containing the product
  6. concentrationconcentrated
  7. filtrationthe solid was filtered
  8. customrecrystallized from toluene

출처 및 근거

ORD 기록
ord-b5414ddf5a2343b081d3026e5e10cc4e
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04743601

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