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Ammonium Chloride → N4-(3-Chloro-4-fluorophenyl)-7-(((3S)-tetrahydro-3-furanyl)oxy)-4,6-quinazolinediamine

HRID 2423010
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HRID 2423010 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:23][C@H:24]4[CH2:28][CH2:27][O:26][CH2:25]4)=[C:17]([N+:20]([O-])=O)[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:5]=[CH:6][C:7]=1[F:8].[Cl-].[NH4+].[H][H]>CN(C=O)C.[Ni]>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:23][C@H:24]4[CH2:28][CH2:27][O:26][CH2:25]4)=[C:17]([NH2:20])[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:5]=[CH:6][C:7]=1[F:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 54376755N-(3-Chloro-4-fluorophenyl)-6-nitro-7-[[(3S)-tetrahydro-3-furanyl]oxy]-4-quinazolinamineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 15606392N4-(3-Chloro-4-fluorophenyl)-7-(((3S)-tetrahydro-3-furanyl)oxy)-4,6-quinazolinediamine

시약·촉매·용매 2

HCID 935Nickel촉매
HCID 6228
Dimethylformamide
용매

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온도
0 °C

실험 절차

100 g of 4-[(3-chloro4-fluorophenyl)amino]-6-nitro-7-((S)-tetrahydrofuran-3-yloxy)-quinazoline are hydrogenated in 400 ml DMF in the presence of 33.1 g Raney nickel and 18.7 g ammonium chloride at 40° C., until the calculated amount of hydrogen has been taken up. The catalyst is filtered off and the filtrate is added dropwise to 1.2 l water. The suspension is stirred for 2.5 h at 0° C., suction filtered and washed with 500 ml of water. The residue is dried overnight at 55° C. under reduced pressure.

후처리

  1. filtrationThe catalyst is filtered off
  2. additionthe filtrate is added dropwise to 1.2 l water
  3. filtrationsuction filtered
  4. washwashed with 500 ml of water
  5. customThe residue is dried overnight at 55° C. under reduced pressure

출처 및 근거

ORD 기록
ord-652aca511bfb4503b257af7ee78bc575
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960546B2

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