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Ethanol → HCID 9861583, 화합물

HRID 603359
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HRID 603359 반응식
[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[CH:5]=[C:4]([F:10])[C:3]=1[N:11]1[C:19]2[C:14](=[CH:15][C:16]([CH3:20])=[CH:17][CH:18]=2)[CH2:13][C:12]1=[O:21].C([OH:24])C>O>[CH3:20][C:16]1[CH:17]=[CH:18][C:19]([NH:11][C:3]2[C:4]([F:10])=[CH:5][C:6]([F:9])=[C:7]([F:8])[C:2]=2[F:1])=[C:14]([CH2:13][C:12]([OH:21])=[O:24])[CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 702EthanolHCID 57952167HCID 57952167, 화합물

생성물 1

HCID 9861583HCID 9861583, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The suspension of 350 mg of N-(2′,3′,4′,6′-tetrafluorophenyl)-5-methyloxindole in 20 ml of ethanol and 5 ml of water is degassed by passing through nitrogen for 1.5 h. Then 260 mg of 30% aqueous sodium hydroxide is added and the mixture is heated to reflux for 6.5 hours. Most of the ethanol is then removed by distillation the mixture is cooled to room temperature followed by the slow addition of 1N hydrochloric acid (1.05 g) to reach a pH of about 3. The precipitate is then filtered, washed with ethanol/water (1:1) and dried in vacuo at room temperature affording the title product.

후처리

  1. customis degassed
  2. additionThen 260 mg of 30% aqueous sodium hydroxide is added
  3. temperaturethe mixture is heated
  4. temperatureto reflux for 6.5 hours
  5. customMost of the ethanol is then removed by distillation the mixture
  6. additionfollowed by the slow addition of 1N hydrochloric acid (1.05 g)
  7. filtrationThe precipitate is then filtered
  8. washwashed with ethanol/water (1:1)
  9. customdried in vacuo at room temperature

출처 및 근거

ORD 기록
ord-ffce5957ed064c9fa254cb475a622631
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07906677B2

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