Sodium Hydroxide → 5-Iodo-2-methoxy-4-methylbenzoic acid

HRID 624308ノート

反応式

HRID 624308 の反応式
[I:1][C:2]1[C:3]([CH3:14])=[CH:4][C:5]([O:12][CH3:13])=[C:6]([CH:11]=1)[C:7]([O:9]C)=[O:8].[OH-].[Na+]>C(O)C>[I:1][C:2]1[C:3]([CH3:14])=[CH:4][C:5]([O:12][CH3:13])=[C:6]([CH:11]=1)[C:7]([OH:9])=[O:8]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 29934724Methyl 5-iodo-2-methoxy-4-methylbenzoate

生成物 1

HCID 468293605-Iodo-2-methoxy-4-methylbenzoic acid収率 76.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of methyl 5-iodo-2-methoxy-4-methylbenzoate (3.0 g, 9.80 mmol) in ethanol (10 ml) in a 50 ml RB flask was added an aqueous solution of NaOH (0.784 g, 19.60 mmol, 1M). The reaction mixture was stirred at room temperature overnight. The solvent was removed under vacuum, the solid filtered and dried to give the titled compound (2.2 g, 74%). LCMS: (ES+) m/z=292 (M+H)+; Column. PUROSPHER@star RP-18 (4×55) mm, 3 μm; Buffer: 20 mM NH4OAc IN WATER; Mphase A: Buffer+MeCN (90+10); Mphase B: Buffer+MeCN (10+90); Flow: 2.5 ml/min Time (min.): 0 2 2.5 3; % B: 0 100 100 0; RT: 1.04 min.

後処理

  1. customThe solvent was removed under vacuum
  2. filtrationthe solid filtered
  3. customdried

出典と根拠

ORDレコード
ord-e27a0f9893b4462caed620253f2a30ad
出典データセット
uspto-grants-2016_04
特許番号
US09303020B2

反応ノート

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