Ammonia → 3-(9,10-Didehydro-12-ethylamino-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

HRID 35217

반응식

HRID 35217 반응식
[C:1]([NH:4][C:5]1[C:19]2=[C:20]3[C:8]([NH:9][CH:10]=[C:11]3[CH2:12][C@@H:13]3[C:18]2=[CH:17][C@H:16]([NH:21][C:22](=[O:28])[N:23]([CH2:26][CH3:27])[CH2:24][CH3:25])[CH2:15][N:14]3[CH3:29])=[CH:7][CH:6]=1)(=O)[CH3:2].[H-].C([Al+]CC(C)C)C(C)C.Cl.N.C(O)(=O)C(C(C(O)=O)O)O>O1CCOCC1.C1(C)C=CC=CC=1.O>[CH2:1]([NH:4][C:5]1[C:19]2=[C:20]3[C:8]([NH:9][CH:10]=[C:11]3[CH2:12][C@@H:13]3[C:18]2=[CH:17][C@H:16]([NH:21][C:22](=[O:28])[N:23]([CH2:24][CH3:25])[CH2:26][CH3:27])[CH2:15][N:14]3[CH3:29])=[CH:7][CH:6]=1)[CH3:2]

참가 물질

9

반응물 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 8752,3-Dihydroxybutanedioic AcidHCID 21225700DiisobutylaluminumhydrideHCID 867423563-(12-Acetylamino-9,10-didehydro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

생성물 1

HCID 867423553-(9,10-Didehydro-12-ethylamino-6-methyl-8alpha-ergolinyl)-1,1-diethylurea수율 70%

시약·촉매·용매 3

HCID 962Water용매HCID 1140Toluene용매HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

200 mg of 3-(12-acetylamino-9,10-didehydro-6-methyl-8α-ergolinyl)-1,1-diethylurea is dissolved in 10 ml of dioxane, combined with 2 ml of 20% diisobutyl aluminum hydride solution in toluene, and heated to 100° C. for 7 hours. The mixture is allowed to cool, then, under cooling, first water, thereafter 2N hydrochloric acid are added thereto, and the solution is rendered alkaline with dilute ammonia, after adding about 1 g of tartaric acid. The mixture is extracted by shaking with methylene chloride, the organic phase is dried and evaporated. The residue is charomatographed as disclosed in Example 7, thus producing 135 mg of 3-(9,10-didehydro-12-ethylamino-6-methyl-8α-ergolinyl)-1,1-diethylurea.

후처리

  1. temperatureto cool
  2. temperatureunder cooling
  3. extractionThe mixture is extracted
  4. customthe organic phase is dried
  5. customevaporated

출처 및 근거

ORD 기록
ord-5ab883efae4c44dbb6f8600b043a3b98
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766128

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