Hydrochloric Acid → HCID 178481601、化合物

HRID 33964

反応式

HRID 33964 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[C:6]([C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)=[C:5]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)[N:4]=[C:3]1SC.C(Cl)Cl.C[OH:31].Cl>O1CCOCC1.[OH-].[Na+]>[OH:31][C:3]1[N:2]([CH3:1])[C:7](=[O:8])[C:6]([C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)=[C:5]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)[N:4]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 21226129Dichloromethane methanolHCID 223466413-methyl-2-methylsulfanyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one

生成物 1

HCID 178481601HCID 178481601、化合物

試薬・触媒・溶媒 2

HCID 14798Sodium Hydroxide溶媒HCID 312751,4-Dioxane溶媒

実験手順

A suspension of 3-methyl-2-methylsulfanyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one (10.1 g, 28.1 mmol) was heated to 100° C. in 100 mL 1,4-dioxane and 60 mL 2.5M sodium hydroxide. After 7 h, TLC (95:5 DCM/MeOH) shows the solution to have no remaining starting material. The reaction was cooled to room temperature and acidified to pH 5 with 5M HCl. The resulting precipitate was collected by filtration, and then suspended in 100 mL hot methanol. The solid was cooled to room temperature then collected by filtration and washed with 100 mL diethylether. The product was air dried overnight to give a pale yellow solid. M+1=330.2.

後処理

  1. filtrationThe resulting precipitate was collected by filtration
  2. temperatureThe solid was cooled to room temperature
  3. filtrationthen collected by filtration
  4. washwashed with 100 mL diethylether
  5. customdried overnight
  6. customto give a pale yellow solid

出典と根拠

ORDレコード
ord-4dcf350333074a329c3813bb192a0da1
出典データセット
uspto-grants-2008_09
特許番号
US07429594B2

関連ノート

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