Hydrochloric Acid → 4-(7-Bromoquinazolin-2-ylamino)-N-(3-(pyrrolidin-1-yl)propyl)benzenesulfonamide

HRID 2079642ノート

反応式

HRID 2079642 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[N:7][C:8](Cl)=[N:9]2)=[CH:4][CH:3]=1.[NH2:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([NH:23][CH2:24][CH2:25][CH2:26][N:27]2[CH2:31][CH2:30][CH2:29][CH2:28]2)(=[O:22])=[O:21])=[CH:16][CH:15]=1.Cl.O1CCOCC1>C(O)(C)C.C(OCC)(=O)C>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[N:7][C:8]([NH:13][C:14]3[CH:15]=[CH:16][C:17]([S:20]([NH:23][CH2:24][CH2:25][CH2:26][N:27]4[CH2:31][CH2:30][CH2:29][CH2:28]4)(=[O:22])=[O:21])=[CH:18][CH:19]=3)=[N:9]2)=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 457900527-Bromo-2-chloroquinazolineHCID 55137112HCID 55137112、化合物

生成物 1

HCID 671016584-(7-Bromoquinazolin-2-ylamino)-N-(3-(pyrrolidin-1-yl)propyl)benzenesulfonamide

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

To a 0.1M suspension of 7-bromo-2-chloroquinazoline in isopropanol was added 4-amino-N-(3-(pyrrolidin-1-yl)propyl)benzenesulfonamide (1.1 eq), followed by the addition of 4.0M HCl in dioxane (1.1 eq). The reaction mixture was heated to 120° C. in an oil bath for 1 h. LCMS showed that reaction was complete under the condition. Ethyl acetate was added to the reaction flask and the mixture was washed with saturated sodium bicarbonate, brine, dried over sodium sulfate and concentrated. Desired product was a yellow color solid. ES/MS m/z 490/492 (MH+).

後処理

  1. customLCMS showed that reaction
  2. washthe mixture was washed with saturated sodium bicarbonate, brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-9f14fbc028ca48d58af18d18daca00cf
出典データセット
uspto-grants-2011_04
特許番号
US07932262B2

反応ノート

読み込み中…