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Ammonia → (17Beta)-13-Ethyl-3-methoxygona-2,5(10)-dien-17-ol

HRID 1077173
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HRID 1077173 반응식
[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C:12]4[CH:13]=[CH:14][C:15]([O:20][CH3:21])=[CH:16][C:17]=4[CH2:18][CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C@@H:4]2[OH:22])[CH3:2].N.[Li].[Cl-].[NH4+]>COCC(O)C.O>[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C:12]4[CH2:13][CH:14]=[C:15]([O:20][CH3:21])[CH2:16][C:17]=4[CH2:18][CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C@@H:4]2[OH:22])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 25517Ammonium ChlorideHCID 66432(17beta)-13-Ethyl-3-methoxygona-1,3,5(10)-trien-17-olHCID 3028194Lithium

생성물 1

HCID 101950(17Beta)-13-Ethyl-3-methoxygona-2,5(10)-dien-17-ol

시약·촉매·용매 2

HCID 962Water용매
HCID 7900
1-Methoxy-2-propanol
용매

실험 절차

To 13β-ethyl-3-methoxy-gona-1,3,5(10)-trien-17β-ol (1.0 g.) in 1-methoxypropan-2-ol (100 cc.) add liquid ammonia (200 cc.), followed by lithium metal (1.2 g.) in small pieces with stirring. After discharge of the blue color add an excess ammonium chloride, followed by water; filter off the crude 13β-ethyl-3-methoxy-gona-2,5(10)-dien-17β-ol and dry, m.p. 98°-104°. No selective ultra-violet absorption beyond 220 mμ; infrared absorption peaks at 3.03, 5.92, 6.01 μ.

후처리

  1. filtrationfilter off the crude 13β-ethyl-3-methoxy-gona-2,5(10)-dien-17β-ol
  2. customdry
  3. customNo selective ultra-violet absorption beyond 220 mμ
  4. custominfrared absorption peaks at 3.03, 5.92, 6.01 μ

출처 및 근거

ORD 기록
ord-e3143b7af7464c89a6c753fe74b87862
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03959322

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