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Water → HCID 84657183, 화합물

HRID 524348
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HRID 524348 반응식
[CH:1]1([S:4][C:5]2[CH:13]=[CH:12][C:8]([C:9]([NH2:11])=O)=[CH:7][CH:6]=2)[CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[CH:1]1([S:4][C:5]2[CH:13]=[CH:12][C:8]([CH2:9][NH2:11])=[CH:7][CH:6]=2)[CH2:2][CH2:3]1
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참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 86711600HCID 86711600, 화합물

생성물 1

HCID 84657183HCID 84657183, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

A solution of 4-cyclopropylsulfanyl-benzamide (preparation 31a, 137 mg, 0.71 mmol) in dry tetrahydrofuran (1.0 mL) is added at 0° C. to a solution of lithium aluminium hydride in tetrahydrofuran (1 M, 2.1 mL, 2.1 mmol). The mixture is stirred at 0° C. for 1 h and heated at reflux for 1 h. The mixture is cooled at room temperature and stirred for 1.5 h. Water is added, and the mixture is extracted twice with dichloromethane. The combined organic layers are dried over Na2SO4 and concentrated under reduced pressure. Yield: 75 mg (60% of theory); ESI mass spectrum: [M+H]+=180; Retention time HPLC: 0.51 min (X011_S03).

후처리

  1. temperatureheated
  2. temperatureat reflux for 1 h
  3. temperatureThe mixture is cooled at room temperature
  4. stirringstirred for 1.5 h
  5. extractionthe mixture is extracted twice with dichloromethane
  6. dry with materialThe combined organic layers are dried over Na2SO4
  7. concentrationconcentrated under reduced pressure
  8. custom0.51 min (X011_S03)

출처 및 근거

ORD 기록
ord-c70b79b8e0c94375b8c6197ef7c4b4c0
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09340507B2

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