Dimethylformamide → HCID 19800031、化合物

HRID 1646871ノート

反応式

HRID 1646871 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 purifed 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. additionThe fractions containing the product
  5. concentrationconcentrated
  6. filtrationthe solid was filtered
  7. customrecrystallized from toluene

出典と根拠

ORDレコード
ord-9e7f6e2fb44e4ca8aa676b47b60a3cfc
出典データセット
uspto-grants-1993_01
特許番号
US05182275

反応ノート

読み込み中…