Ammonium Hydroxide → HCID 178433360、化合物

HRID 1710809ノート

反応式

HRID 1710809 の反応式
I.[Cl:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH:5]([CH3:15])[NH:6][C:7](SC)=[N:8]2.[OH-].[NH4+:17]>C(#N)C.C(O)(C(F)(F)F)=O>[Cl:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH:5]([CH3:15])[NH:6][C:7]([NH2:17])=[N:8]2

参加物

5

反応物 2

HCID 14923Ammonium HydroxideHCID 178503338HCID 178503338、化合物

生成物 1

HCID 178433360HCID 178433360、化合物収率 62%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒2 回HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
130 °C

実験手順

5-Chloro-4-methyl-2-methylsulfanyl-3,4-dihydro-quinazoline hydroiodide (100 mg, 0.28 mmol) was suspended in a mixture of ammonium hydroxide (1 ml, 25% in H2O) and acetonitrile (1 ml) and heated in a microwave oven to 130° C. (15 min) and subsequently to 170° C. (30 min). The title compound (35 mg, 62%) was isolated from the reaction mixture by preparative, reverse-phase HPLC (YMC CombiPrep C18 column 50×20 mm, solvent gradient 5-95% CH3CN in 0.1% TFA(aq) over 6.0 min, λ=230 nm, flow rate 40 ml/min) as a white solid.

後処理

  1. customsubsequently to 170° C.
  2. custom(30 min)

出典と根拠

ORDレコード
ord-2b447037860e40dba23ae0b94373cea9
出典データセット
uspto-grants-2010_09
特許番号
US07790732B2

反応ノート

読み込み中…