Methanol → 3-(2-Hydroxy-4-methoxy-5-thiocyanato-phenyl)-propionic acid methyl ester

HRID 984114

反応式

HRID 984114 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][C:9](=[O:13])[O:10]2)=[CH:5][CH:4]=1.[C:14]([S-:16])#[N:15].[K+].BrBr.[CH3:20][OH:21]>>[CH3:20][O:21][C:9](=[O:13])[CH2:8][CH2:7][C:6]1[CH:5]=[C:4]([S:16][C:14]#[N:15])[C:3]([O:2][CH3:1])=[CH:12][C:11]=1[OH:10]

参加物

5

反応物 4

HCID 887MethanolHCID 24408BromineHCID 516872Potassium thiocyanateHCID 123898377-Methoxychroman-2-one

生成物 1

HCID 207659993-(2-Hydroxy-4-methoxy-5-thiocyanato-phenyl)-propionic acid methyl ester

実験手順

Compound 14A (3 g), KSCN (4.9 g) were dissolved in MeOH (125 mL) at 0° C., Br2 (3 g) was added, then stirred for 2 h. The reaction mixture was quenched with water (200 mL) and ethyl acetate (200 mL). The ethyl acetate was separated and washed with water, brine, dried (MgSO4), concentrated, to afford compound 14B (3.5 g). mp 105-016° C.; MS: 268 (M+1)+. Preparation of 6-Mercapto-7-methoxy-chroman-2-ol (Compound 14C)

後処理

  1. customThe reaction mixture was quenched with water (200 mL) and ethyl acetate (200 mL)
  2. customThe ethyl acetate was separated
  3. washwashed with water, brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-48c920a6ff2048748cf5783424bcecc1
出典データセット
uspto-grants-2005_03
特許番号
US06867224B2

関連ノート

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