Lithium Hydroxide → HCID 25744650, 화합물

HRID 84191노트

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HRID 84191 반응식
[Li+].[OH-].C[O:4][C:5]([C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[N:12]([S:16]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:18])=[O:17])[CH2:11][CH2:10]2)=[O:6]>O1CCOCC1>[C:19]1([S:16]([N:12]2[C:13]3[C:9](=[CH:8][C:7]([C:5]([OH:6])=[O:4])=[CH:15][CH:14]=3)[CH2:10][CH2:11]2)(=[O:18])=[O:17])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 31756086Methyl 1-(Phenylsulfonyl)indoline-5-carboxylate

생성물 1

HCID 25744650HCID 25744650, 화합물수율 93.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
40 °C

실험 절차

1M LiOH aqueous solution (2.4 ml, 2.40 mmol) was added to a solution of 11 (0.38 g, 1.20 mmol) in dioxane (15 mL). The reaction mixture was stirred at 40° C. overnight and then was concentrated under reduced pressure. The residue was dissolved in water and concentrated HCl was added up to acidic pH to give the precipitation, which was dried by vacuum to afford 16 (0.34 g). 1H NMR (500 MHz, CD3OD): δ 2.97 (t, J=8.6 Hz, 2H), 3.99 (t, J=8.6 Hz, 2H), 7.51-7.54 (m, 2H), 7.61-7.64 (m, 2H), 7.74 (s, 1H), 7.84-7.88 (m, 3H).

후처리

  1. concentrationwas concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in water
  3. additionconcentrated HCl was added up to acidic pH
  4. customto give
  5. customthe precipitation, which
  6. customwas dried by vacuum

출처 및 근거

ORD 기록
ord-b7a24551a1f34319a5084d47e707ac02
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846748B2

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