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Trimethylsilyldiazomethane → Methyl 2-amino-4-methoxybenzoate

HRID 241033
ノート
印刷プレビュー

反応式

HRID 241033 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH2:12])[C:6](=[CH:10][CH:11]=1)[C:7]([OH:9])=[O:8].[CH3:13][Si](C=[N+]=[N-])(C)C>CO.O1CCCC1>[NH2:12][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[CH:11]=[CH:10][C:6]=1[C:7]([O:9][CH3:13])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 167693TrimethylsilyldiazomethaneHCID 3510102-Amino-4-methoxybenzoic acid

生成物 1

HCID 12919999Methyl 2-amino-4-methoxybenzoate

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-methoxyanthranilic acid (5.0 g, 30.0 mmol) in a mixture of 10% methanol in tetrahydrofuran (100 mL) was added dropwise (trimethylsilyl)diazomethane (2.0 M solution in diethyl ether, 18.0 mL, 36.0 mmol) at 0° C. The reaction mixture was stirred for 16 hours at room temperature then quenched by the addition of glacial acetic acid (0.1 mL). The reaction mixture was concentrated and the residue was partitioned between saturated sodium bicarbonate (50 mL) and ethyl acetate (250 mL). The organic layer was separated and washed with water (50 mL), saturated sodium bicarbonate (50 mL) and brine (50 mL), dried over sodium sulfate, filtered and concentrated to give methyl 2-amino-4-methoxybenzoate as an oil (5.4 g, quantitative). MS (EI) for C9H11NO3: 182 (MH+).

後処理

  1. customthen quenched by the addition of glacial acetic acid (0.1 mL)
  2. concentrationThe reaction mixture was concentrated
  3. customthe residue was partitioned between saturated sodium bicarbonate (50 mL) and ethyl acetate (250 mL)
  4. customThe organic layer was separated
  5. washwashed with water (50 mL), saturated sodium bicarbonate (50 mL) and brine (50 mL)
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-f743523be02a438aa262fe6cef8e59c1
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08648066B2

反応ノート

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