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1,2-Dichloroethane → HCID 9818690, 화합물

HRID 1586139
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HRID 1586139 반응식
[CH2:1]([N:3]1[C:7]2=[N:8][C:9]3[C:14]([C:15]([NH:16][CH2:17][CH:18]4[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]4)=[C:6]2[CH:5]=[N:4]1)=[CH:13][C:12]([O:24]C)=[CH:11][CH:10]=3)[CH3:2].B(Br)(Br)Br.ClCCCl.[OH-].[Na+]>O>[CH2:1]([N:3]1[C:7]2=[N:8][C:9]3[C:14]([C:15]([NH:16][CH2:17][CH:18]4[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]4)=[C:6]2[CH:5]=[N:4]1)=[CH:13][C:12]([OH:24])=[CH:11][CH:10]=3)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 14798Sodium HydroxideHCID 25134Boron tribromideHCID 9884287HCID 9884287, 화합물

생성물 1

HCID 9818690HCID 9818690, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1-ethyl-6-methoxy-N-(cyclohexylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine (5.4 g, 0.016 mol), boron tribromide (48 ml, 0.048 mol) and 1,2-dichloroethane (250 ml) is stirred at room temperature overnight. The reaction mixture is stirred with 1 volume of water, made basic with NaOH, and the layers are separated. The basic layer is acidified with acetic acid and the yellow precipitate that forms is collected by filtration, washed with water and dried. The product is recrystallized from hot acetonitrile/methanol to afford 1-ethyl-6-hydroxy-N-(cyclohexylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine, as a yellow powder, m.p. 223°-224° C.

후처리

  1. customthe layers are separated
  2. filtrationthe yellow precipitate that forms is collected by filtration
  3. washwashed with water
  4. customdried
  5. customThe product is recrystallized from hot acetonitrile/methanol

출처 및 근거

ORD 기록
ord-405a393f160a4255831ccc62085e6a7f
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05942520

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