Dimethylformamide → HCID 19800031、化合物

HRID 1252417ノート

反応式

HRID 1252417 の反応式
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

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 14209243HCID 14209243、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 19800031HCID 19800031、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b5414ddf5a2343b081d3026e5e10cc4e
出典データセット
uspto-grants-1988_05
特許番号
US04743601

反応ノート

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