4-Chloro-2-fluorobenzoyl chloride → HCID 21905770, 화합물

HRID 1246791

반응식

HRID 1246791 반응식
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)[C:3]=1[NH2:16].[Cl:17][C:18]1[CH:26]=[CH:25][C:21]([C:22](Cl)=[O:23])=[C:20]([F:27])[CH:19]=1>N1C=CC=CC=1.C(O)C>[Cl:17][C:18]1[CH:26]=[CH:25][C:21]([C:22]([NH:16][C:3]2[C:2]([Cl:1])=[N:7][CH:6]=[N:5][C:4]=2[NH:8][C:9]2[CH:10]=[CH:11][C:12]([Cl:15])=[CH:13][CH:14]=2)=[O:23])=[C:20]([F:27])[CH:19]=1

참가 물질

5

반응물 2

HCID 27736014-Chloro-2-fluorobenzoyl chlorideHCID 167263116-Chloro-N~4~-(4-chlorophenyl)pyrimidine-4,5-diamine

생성물 1

HCID 21905770HCID 21905770, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 1049Pyridine용매

실험 절차

6-Chloro-N4-(4-chlorophenyl)-pyrimidine-4,5-diamine I-(1A-1)a (6.6 g, 26 mmol) in pyridine (30 ml) was cooled to 0° C. and to it was added 4-chloro-2-fluorobenzoyl chloride (5 g, 26 mmol). The reaction was then allowed to warm to ambient temperature overnight. The heterogeneous reaction was diluted with ethanol (50 ml) and the resulting solid collected by filtration. The solids were slurried in toluene, which was then removed under reduced pressure to remove residual ethanol. The solid was slurried in diethyl ether and then collected by filtration to give I-(7A-91)a (8.3 g, 78%): +ACPI MS (M+1) 409.0; 1H NMR (400 MHz, CD3OD) δ 10.60 (s, 1H), 10.10 (s, 1H), 9.19 (s, 1H), 8.74 (t, J=8.1 Hz, 1H), 8.46–8.40 (m, 3H), 8.28 (dd, J=8.7, 2.1 Hz, 1H), 8.20 (d, J=8.7 Hz, 2H).

후처리

  1. customThe heterogeneous reaction
  2. filtrationthe resulting solid collected by filtration
  3. customwhich was then removed under reduced pressure
  4. customto remove residual ethanol
  5. filtrationcollected by filtration
  6. customto give I-(7A-91)a (8.3 g, 78%)

출처 및 근거

ORD 기록
ord-1800146ac7c349e69101ea3ed85714e4
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129239B2

연결된 노트

불러오는 중…