Water → HCID 12600751, 화합물

HRID 1078368노트

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HRID 1078368 반응식
[C:1]1([C:7]2[S:11][N:10]=[C:9](OCCCCl)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O>ClCCl>[C:1]1([C:7]2[S:11][N:10]=[CH:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 22902407HCID 22902407, 화합물

생성물 1

HCID 12600751HCID 12600751, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
65 °C

실험 절차

0.85 g of the product obtained above were reacted with 0.7 g of 3-(5-phenyl-1,2,4-thiadiazole-3-yloxy)-propyl chloride [for preparation, see Example 54 B)] and the reaction mixture was stirred for 10.5 hours at 65° C. Then the reaction mixture was dissolved in dichloromethane and the solution shaken with water. The dichloromethane phase was separated, dried, and concentrated. The crude product obtained was purified by medium-pressure chromatography on fine-grained silica gel (Lichroprep Si 60®) using 9:1 ethyl acetate/methanol as the eluent. 0.5 g of 3-{3-[N-[2-(4-(2-trimethylsilyl)-ethoxymethoxy)-3-methoxyphenyl)-ethyl]-N-methylamino]-propyloxy)-5-phenyl-1,2,4-thiadiazole were obtained as a colorless oil.

후처리

  1. customfor preparation
  2. customThe dichloromethane phase was separated
  3. customdried
  4. concentrationconcentrated
  5. customThe crude product obtained
  6. customwas purified by medium-pressure chromatography on fine-grained silica gel (Lichroprep Si 60®)

출처 및 근거

ORD 기록
ord-3b030090e8de4f59a0c1fc5116126ae5
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05547967

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