Diazomethane → Methyl 4-bromo-2-chloro-6-methylbenzoate

HRID 2427492ノート

反応式

HRID 2427492 の反応式
[Br:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:5]([C:6]([OH:8])=[O:7])=[C:4]([Cl:12])[CH:3]=1.[N+](=[CH2:15])=[N-]>C(OCC)(=O)C.C(OCC)C>[CH3:15][O:7][C:6](=[O:8])[C:5]1[C:9]([CH3:11])=[CH:10][C:2]([Br:1])=[CH:3][C:4]=1[Cl:12]

参加物

5

反応物 2

HCID 9550DiazomethaneHCID 566042464-Bromo-2-chloro-6-methylbenzoic acid

生成物 1

HCID 45480505Methyl 4-bromo-2-chloro-6-methylbenzoate収率 113%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8857Ethyl Acetate溶媒

実験手順

4-Bromo-2-chloro-6-methylbenzoic acid (1.10 g, 4.41 mmol) was dissolved in ethyl acetate (15 mL). A solution of diazomethane in diethyl ether was added until the yellow colour persisted. After fifteen minutes the reaction was quenched with acetic acid. After one hour, the mixture was washed with saturated sodium bicarbonate and brine, dried over magnesium sulfate, filtered and concentrated to provide the title compound as a yellow oil (1.31 g, 113%). 1H NMR CDCl3: 7.43 (s, 1H), 7.31 (s, 1H), 3.94 (s, 3H), 2.33 (s, 3H).

後処理

  1. customAfter fifteen minutes the reaction was quenched with acetic acid
  2. washthe mixture was washed with saturated sodium bicarbonate and brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-5ed3020889ad43c7bf69b2e437b5e85d
出典データセット
uspto-grants-2011_06
特許番号
US07968570B2

反応ノート

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