Potassium Carbonate → HCID 20041122, 화합물

HRID 1762556노트

반응식

HRID 1762556 반응식
[OH:1][CH:2]([CH2:16][OH:17])[CH2:3][N:4]1[C:12]2[C:11](=[O:13])[NH:10][C:9](=[O:14])[N:8]([CH3:15])[C:7]=2[N:6]=[CH:5]1.Cl[CH2:19][CH2:20][CH2:21][CH2:22][C:23]([OH:26])([CH3:25])[CH3:24].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[OH:1][CH:2]([CH2:16][OH:17])[CH2:3][N:4]1[C:12]2[C:11](=[O:13])[N:10]([CH2:19][CH2:20][CH2:21][CH2:22][C:23]([OH:26])([CH3:25])[CH3:24])[C:9](=[O:14])[N:8]([CH3:15])[C:7]=2[N:6]=[CH:5]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 3616685AC1MUDJSHCID 137476791-Chloro-5-hydroxy-5-methylhexane

생성물 1

HCID 20041122HCID 20041122, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

A mixture of 18 g (0.075 mol) of the xanthine compound from stage (a), 12.5 g (0.083mol) of 1-chloro-5-hydroxy-5-methylhexane (Example 1a) and 11.5 g (0.083 mol) of potassium carbonate in 500 ml of dimethylformamide is stirred for 18 hours at 110° C., after which the hot mixture is filtered and the filtrate is concentrated in vacuo. The oily crude product, which gradually crystallizes through, can advantageously be purified by filtration over a silica gel column using a chloroform/methanol (10:1) solvent mixture, followed by a final recrystallization from ethyl acetate with the addition of petroleum ether, at the boil.

후처리

  1. filtrationafter which the hot mixture is filtered
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe oily crude product, which gradually crystallizes through,
  4. filtrationcan advantageously be purified by filtration over a silica gel column
  5. customrecrystallization from ethyl acetate
  6. additionwith the addition of petroleum ether

출처 및 근거

ORD 기록
ord-4c5596507ba14ffba2e2f104168b3061
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04833146

반응 노트

불러오는 중…