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Ethanol → (R)-N4-(3-Chloro-4-fluorophenyl)-7-((tetrahydrofuran-3-yl)oxy)quinazoline-4,6-diamine

HRID 1929242
ノート
印刷プレビュー

反応式

HRID 1929242 の反応式
[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].C(O)C.O>[Fe].C(O)(=O)C>[NH2:20][C:17]1[CH:18]=[C:19]2[C:14](=[CH:15][C:16]=1[O:23][C@@H:24]1[CH2:28][CH2:27][O:26][CH2:25]1)[N:13]=[CH:12][N:11]=[C:10]2[NH:9][C:4]1[CH:5]=[CH:6][C:7]([F:8])=[C:2]([Cl:1])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 702EthanolHCID 962WaterHCID 66936816(R)-N-(3-Chloro-4-fluorophenyl)-6-nitro-7-((tetrahydrofuran-3-yl)oxy)quinazolin-4-amine

生成物 1

HCID 66936486(R)-N4-(3-Chloro-4-fluorophenyl)-7-((tetrahydrofuran-3-yl)oxy)quinazoline-4,6-diamine

試薬・触媒・溶媒 2

HCID 23925Iron触媒
HCID 176
Acetic Acid
溶媒

実験手順

A mixture of 12.80 g of 4-[(3-chloro-4-fluorophenyl)amino]-6-nitro-7-((R)-tetrahydrofuran-3-yloxy)quinazoline, 200 ml of ethanol, 100 ml of water, and 17.20 ml of glacial acetic acid is heated to reflux temperature. Then a total of 7.00 g of iron powder is added in batches. The reaction mixture is refluxed for about four hours and then cooled to ambient temperature overnight. For working up, the reaction mixture is evaporated using the rotary evaporator. The residue is taken up in methylene chloride/methanol (9:1), mixed with 20 ml of concentrated ammonia solution and filtered through a layer of silica gel. It is washed with copious amounts of methylene chloride/methanol (9:1) and the combined filtrates are evaporated down. The residue is stirred with diethylether and suction filtered. Yield: 8.59 g (73% of theory); mass spectrum (ESI−): m/z=373, 375 [M−H]−; Rf value: 0.27 (silica gel, ethyl acetate/methanol=9:1).

後処理

  1. temperatureis heated
  2. temperatureto reflux temperature
  3. temperatureThe reaction mixture is refluxed for about four hours
  4. customthe reaction mixture is evaporated
  5. customthe rotary evaporator
  6. additionmixed with 20 ml of concentrated ammonia solution
  7. filtrationfiltered through a layer of silica gel
  8. washIt is washed with copious amounts of methylene chloride/methanol (9:1)
  9. customthe combined filtrates are evaporated down
  10. filtrationfiltered

出典と根拠

ORDレコード
ord-de015d718aaa420e876ded7f765af087
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE043431E1

反応ノート

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