2-Methyl-3-(4-morpholinyl)benzoic acid → HCID 67112254、化合物

HRID 594990ノート

反応式

HRID 594990 の反応式
[CH3:1][C:2]1[C:10]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5]>C1COCC1>[CH3:1][C:2]1[C:10]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)=[CH:9][CH:8]=[CH:7][C:3]=1[CH2:4][OH:5]

参加物

3

反応物 1

HCID 71484262-Methyl-3-(4-morpholinyl)benzoic acid

生成物 1

HCID 67112254HCID 67112254、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

2-methyl-3-morpholinobenzoic acid (0.5 g, 2.26 mmol) was dissolved in dry THF (12 mL) under Nitrogen and the solution was cooled at 0° C. with an ice bath. A solution of BH3 (1M in THF, 3.39 mL, 3.39 mmol) was added dropwise and the reaction was allowed to reach rt overnight. The mixture was quenched with NH4Cl (sat. solution, 2 mL) and diluted with ethyl acetate (20 mL). The organics were separated, washed with water (10 mL) and brine (10 mL) and dried over Na2SO4. The filtered solution was evaporated under vacuum to give (2-methyl-3-morpholinophenyl)methanol as a crude oil which crystallized over 2 h (0.5 g, quantitative).

後処理

  1. customThe mixture was quenched with NH4Cl (sat. solution, 2 mL)
  2. additiondiluted with ethyl acetate (20 mL)
  3. customThe organics were separated
  4. washwashed with water (10 mL) and brine (10 mL)
  5. dry with materialdried over Na2SO4
  6. customThe filtered solution was evaporated under vacuum

出典と根拠

ORDレコード
ord-f047ba796cbd4cbfafe3a0c778ee1b84
出典データセット
uspto-grants-2016_01
特許番号
US09242987B2

反応ノート

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