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Triethylamine → HCID 18953476, 화합물

HRID 1491613
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HRID 1491613 반응식
BrBr.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[O:22]1[CH2:27][CH2:26][N:25]([C:28]2[C:37]3[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=3)[N:31]3[CH:38]=[N:39][C:40]([C:41]([NH2:43])=O)=[C:30]3[N:29]=2)[CH2:24][CH2:23]1.C(N(CC)CC)C>C(Cl)Cl>[C:41]([C:40]1[N:39]=[CH:38][N:31]2[C:32]3[C:37](=[CH:36][CH:35]=[CH:34][CH:33]=3)[C:28]([N:25]3[CH2:26][CH2:27][O:22][CH2:23][CH2:24]3)=[N:29][C:30]=12)#[N:43]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 24408BromineHCID 18953480HCID 18953480, 화합물

생성물 1

HCID 18953476HCID 18953476, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Bromine (0.15 ml) was added dropwise to a solution of triphenylphosphine (0.8 g) in 15 ml of methylene chloride at 5° C. 5-morpholino-imidazo[1,5-a]quinazoline-3carboxamide (0.5 g) and triethylamine (0.83 ml) were added to the solution. The resulting reaction mixture was stirred at room temperature for 3 hours and evaporated in vacuo. Ethyl acetate (10 ml) was added to the residue and crude crystals of the title compound were isolated by filtration. The dried crystals were dissolved in acetone (30 ml) and an excess of hydrogen chloride in diethyl ether was added separating the hydrochloride of the title compound as beige crystals. M.p. 225°-228° C. Yield 0.3 g.

후처리

  1. customThe resulting reaction mixture
  2. customevaporated in vacuo
  3. additionEthyl acetate (10 ml) was added to the residue

출처 및 근거

ORD 기록
ord-fa8839f31cd94e42b67582cedcb7390a
출처 데이터셋
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05371080

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