Hydrochloric Acid → HCID 10630901、化合物

HRID 19372

反応式

HRID 19372 の反応式
[CH3:1][Mg]Br.COC(=O)[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([OH:14])[CH:9]=1.C([O:19][CH2:20][CH3:21])(=O)C.Cl>O1CCCC1.O>[OH:14][C:10]([CH3:11])([CH3:1])[CH2:9][C:8]1[CH:7]=[C:20]([OH:19])[CH:21]=[CH:12][CH:13]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 39129Methyl 3-HydroxyphenylacetateHCID 178418573HCID 178418573、化合物

生成物 1

HCID 10630901HCID 10630901、化合物収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of methyl magnesium bromide (3 M, 12 mL, 36.06 mmol) cooled to 0° C. was added tetrahydrofuran (10 mL) and (3-hydroxy-phenyl)-acetic acid methyl ester (1 g, 6.01 mmol) as a solution in tetrahydrofuran (5 mL). The resulting mixture was warmed to room temperature stirred for 30 min and then poured carefully into a biphasic mixture of ethyl acetate and water. The water layer was made acidic (pH=1) with 1N aqueous hydrochloric acid and extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo which afforded 3-(2-hydroxy-2-methyl-propyl)-phenol (1 g, 100%) as a white solid.

後処理

  1. extractionextracted twice with ethyl acetate
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo which

出典と根拠

ORDレコード
ord-deeeda5aef424b77a2cee8a8fc33472c
出典データセット
uspto-grants-2010_06
特許番号
US07741327B2

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