Hydrochloric Acid → HCID 89809360、化合物

HRID 522711

反応式

HRID 522711 の反応式
[OH:1][CH2:2][C:3](=O)[CH3:4].[NH2:6][C:7]1[C:12]([CH:13]=O)=[CH:11][N:10]=[C:9]([S:15][CH3:16])[N:8]=1.[OH-].[Na+].Cl>O.CCO.O.CCO>[CH3:4][C:3]1[C:2]([OH:1])=[CH:13][C:12]2[CH:11]=[N:10][C:9]([S:15][CH3:16])=[N:8][C:7]=2[N:6]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 8299HydroxyacetoneHCID 14798Sodium HydroxideHCID 2957694-Amino-2-(methylsulfanyl)pyrimidine-5-carbaldehyde

生成物 1

HCID 89809360HCID 89809360、化合物収率 56%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒2 回HCID 19096565Water ethanol溶媒

実験手順

Add 1-hydroxypropan-2-one (24.3 mL, 355 mmol) and 4-amino-2-(methylthio)pyrimidine-5-carbaldehyde (50 g, 296 mmol) to a solution of sodium hydroxide (23.64 g, 591 mmol) and water (200 mL). Add EtOH (600 mL) to the suspension and stir at RT overnight. Slowly add a solution of concentrated HCl (50 mL) in water (350 mL). Add 1:1 EtOH/H2O (100 mL) and collect the solids by filtration. Wash the solids with 1:1 EtOH/H2O (250 mL), ice cold EtOH (4×25 mL) and hexanes (2×250 mL). Dry in the vacuum oven at 30-35° C. to provide the title compound as a tan solid (34 g, 56% yield). MS (m/z): 208.1 (M+1).

後処理

  1. customcollect the solids
  2. filtrationby filtration
  3. washWash the solids with 1:1 EtOH/H2O (250 mL), ice cold EtOH (4×25 mL) and hexanes (2×250 mL)
  4. customDry in the vacuum oven at 30-35° C.

出典と根拠

ORDレコード
ord-3eb8ef251cf0428a967a2a9b4665fc7f
出典データセット
uspto-grants-2016_05
特許番号
US09334267B2

関連ノート

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