Sodium Hydroxide → HCID 11728935, 화합물

HRID 1637206노트

반응식

HRID 1637206 반응식
[OH-].[Na+].[C:3]1([S:9][C:10]2[C:11]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]4[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=4)=[CH:20][C:12]=3[S:13][C:14]=2[C:15]([O:17]CC)=[O:16])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>O1CCOCC1>[C:3]1([S:9][C:10]2[C:11]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]4[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=4)=[CH:20][C:12]=3[S:13][C:14]=2[C:15]([OH:17])=[O:16])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 9931973HCID 9931973, 화합물

생성물 1

HCID 11728935HCID 11728935, 화합물수율 79.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

Sodium hydroxide (0.5 ml of 2M in water) was added to a solution of ethyl 3-(phenylsulfanyl)-6-(3-pyridylmethoxy)benzo[b]thiophene-2-carboxylate (Example 1, 190 mg, 0.45 mmol) in 1,4-dioxane, and the mixture heated to 60° C. for 4 hours. The solvents were removed under reduced pressure, and the residue was dissolved in water (15 ml) and washed with ethyl acetate (25 ml). The aqueous layer was separated and acidified by dropwise addition of acetic acid until a white solid precipitated. The solid was isolated by filtration and dried under vacuo to give the title compound as a colourless solid (140 mg).

후처리

  1. customThe solvents were removed under reduced pressure
  2. dissolutionthe residue was dissolved in water (15 ml)
  3. washwashed with ethyl acetate (25 ml)
  4. customThe aqueous layer was separated
  5. additionacidified by dropwise addition of acetic acid until a white solid
  6. customprecipitated
  7. customThe solid was isolated by filtration
  8. customdried under vacuo

출처 및 근거

ORD 기록
ord-3e8b41e8ee1d4fa68f1ba0a8a7e1524d
출처 데이터셋
uspto-grants-2000_03
특허 번호
US06040309

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