Ammonium Hydroxide → HCID 178456164, 화합물

HRID 1199667노트

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HRID 1199667 반응식
[CH:1]([N:4]1[C:18]2[C:19]3[C:6]([CH2:7][C@@H:8]4[C@@H:13]([C:14]=3[CH:15]=[CH:16][CH:17]=2)[CH2:12][C@@H:11]([C:20]([OH:22])=O)[CH2:10][N:9]4[CH3:23])=[CH:5]1)([CH3:3])[CH3:2].C(N1C=CN=C1)(N1C=CN=C1)=O.Cl.Cl.[NH2:38][CH2:39][CH2:40][C:41]1[N:45]=[CH:44][NH:43][CH:42]=1.[OH-].[NH4+]>CN(C)C=O.C(N(CC)CC)C>[NH:43]1[CH:42]=[C:41]([CH2:40][CH2:39][NH:38][C:20]([C@@H:11]2[CH2:12][C@H:13]3[C@@H:8]([CH2:7][C:6]4[C:19]5[C:18](=[CH:17][CH:16]=[CH:15][C:14]3=5)[N:4]([CH:1]([CH3:3])[CH3:2])[CH:5]=4)[N:9]([CH3:23])[CH2:10]2)=[O:22])[N:45]=[CH:44]1

참가 물질

7

반응물 4

HCID 14923Ammonium HydroxideHCID 682631,1'-CarbonyldiimidazoleHCID 1825776-Methyl-1-(propan-2-yl)ergoline-8-carboxylic acidHCID 178478691HCID 178478691, 화합물

생성물 1

HCID 178456164HCID 178456164, 화합물수율 53%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8471Triethylamine용매

실험 절차

To a mixture of 3.5 g of (8β)-1-isopropyl-6-methylergoline-8-carboxylic acid in 80 ml of dimethylformamide were added 2.27 g of 1,1'-carbonyldiimidazole. After stirring for 3 hours at room temperature, the mixture was added dropwise to a solution of 2.27 g of histamine dihydrochloride in 100 ml of dimethylformamide to which 3.6 ml of triethylamine had been added. The reaction mixture was stirred at room temperature overnight and then poured into 2 liters of ice water to which 5 ml of ammonium hydroxide had been added. The resulting precipitate was recovered by filtration. The solid material was crystallized from methanol/water to provide 2.41 g of the desired title product hemihydrate as a light pink powder, m.p. 83°-86° C.

후처리

  1. additionhad been added
  2. stirringThe reaction mixture was stirred at room temperature overnight
  3. additionhad been added
  4. filtrationThe resulting precipitate was recovered by filtration
  5. customThe solid material was crystallized from methanol/water

출처 및 근거

ORD 기록
ord-2ec453b8ddc343e394623130d757e506
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04902691

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