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Pyridine → 17beta-(1-Oxo-3-methylbutyl)-6-azaandrost-4-en-3-one

HRID 1077595
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HRID 1077595 반응식
[C:1]([C@H:4]1[CH2:12][CH2:11][C@H:10]2[C@H:13]3[C@H:23]([CH2:24][CH2:25][C@:5]12[CH2:6]C(O)=O)[C@:21]1([CH3:22])[C:16](=[CH:17][C:18](=[O:26])[CH2:19][CH2:20]1)[N:15](C(C)(C)C)[CH2:14]3)(O)=[O:2].N1C=CC=CC=1.S(Cl)(Cl)=O.[CH2:41]([Mg]Br)[CH:42]([CH3:44])[CH3:43]>C1(C)C=CC=CC=1.CN(C)C=O>[O:2]=[C:1]([C@H:4]1[CH2:12][CH2:11][C@H:10]2[C@H:13]3[C@H:23]([CH2:24][CH2:25][C@:5]12[CH3:6])[C@:21]1([CH3:22])[C:16](=[CH:17][C:18](=[O:26])[CH2:19][CH2:20]1)[NH:15][CH2:14]3)[CH2:41][CH:42]([CH3:44])[CH3:43]
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참가 물질

7

반응물 4

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 8674903417beta-Carboxy-6-t-butylcarboxy-6-azaandrost-4-en-3-oneHCID 178418816HCID 178418816, 화합물

생성물 1

HCID 1006692717beta-(1-Oxo-3-methylbutyl)-6-azaandrost-4-en-3-one

시약·촉매·용매 2

HCID 1140
Toluene
용매
HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

Alternatively, a solution of 17β-carboxy-6-t-butylcarboxy-6-azaandrost-4-en-3-one (260 mg, 0.62 mmol), example 3, Part F, is dissolved in toluene (10 mL) and treated with pyridine (3 eq) and catalytic dimethylformamide, cooled to 0° C., and thionyl chloride added (80 μL, 1.10 mmol). The reaction is then allowed to warm to room temperature and is stirred for 1 hr. The solids are then removed by filtration, the solution concentrated, the resulting crude acid chloride dissolved in THF (6 mL), CuL added (120 mg, 0.62 mmol), cooled to -78° C. and treated with isobutylmagnesium bromide (2.0M in diethyl ether, 0.5 mL, 1 mmol). The reaction is allowed to warm to room temperature, stirred for 30 min and is worked up as in Part C above to give 17β-(1-oxo-3-methylbutyl)-6-azaandrost-4-en-3-one.

후처리

  1. temperatureto warm to room temperature
  2. customThe solids are then removed by filtration
  3. concentrationthe solution concentrated
  4. dissolutionthe resulting crude acid chloride dissolved in THF (6 mL)
  5. additionCuL added (120 mg, 0.62 mmol)
  6. temperaturecooled to -78° C.
  7. temperatureto warm to room temperature
  8. stirringstirred for 30 min

출처 및 근거

ORD 기록
ord-c09b852582a342669d6e1f5208b9bc31
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05543406

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