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Hydrazine hydrate (1:1) → HCID 19609556, 화합물

HRID 1029527
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HRID 1029527 반응식
O.[NH2:2][NH2:3].[CH3:4][C:5]([C:8]1[CH:9]=[C:10]([S:19][CH2:20][CH2:21][C:22]([O:24]C)=O)[CH:11]=[C:12]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:13]=1[OH:14])([CH3:7])[CH3:6]>CO.C(OCC)(=O)C>[CH3:4][C:5]([C:8]1[CH:9]=[C:10]([S:19][CH2:20][CH2:21][C:22]([NH:2][NH2:3])=[O:24])[CH:11]=[C:12]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:13]=1[OH:14])([CH3:7])[CH3:6]
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 13531084HCID 13531084, 화합물

생성물 1

HCID 19609556HCID 19609556, 화합물수율 68.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

Hydrazine monohydrate (16 mL, 324 mmol) is added to a room temperature solution of methyl 3-[[3,5-bis-(1,1-dimethylethyl)-4-hydroxyphenyl]thio]propanoate (3.5 g, 10.8 mMol) in methanol (110 mL). The reaction mixture is heated at reflux for 2 hours, then cooled, diluted with ethyl acetate and washed six times with water and once with brine. Drying the organic phase over magnesium sulfate and evaporation provides a crude solid which is chromatographed on a column of silica with methanol/chloroform (5/95) to afford 2.4 g (64%) of 3-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]thio]propanoic acid hydrazide, mp 107.0°-110.0° C.

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for 2 hours
  3. temperaturecooled
  4. washwashed six times with water
  5. customDrying the organic phase
  6. customover magnesium sulfate and evaporation
  7. customprovides a crude solid which
  8. customis chromatographed on a column of silica with methanol/chloroform (5/95)

출처 및 근거

ORD 기록
ord-abe3f67bbbc24ea38d9e2c3ceced520c
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05102897

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