Acetyl chloride → HCID 44359309、化合物

HRID 551778ノート

反応式

HRID 551778 の反応式
Cl.[NH2:2][CH2:3][CH:4]([C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[CH:9]=[CH:8][CH:7]=1)[OH:5].C(=O)([O-])[O-].[K+].[K+].[C:24](Cl)(=[O:26])[CH3:25]>O.C(OCC)(=O)C>[OH:5][CH:4]([C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[CH:9]=[CH:8][CH:7]=1)[CH2:3][NH:2][C:24](=[O:26])[CH3:25]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 11430Potassium CarbonateHCID 445416702-Amino-1-(7-methoxy-1-naphthyl)ethanol hydrochloride

生成物 1

HCID 44359309HCID 44359309、化合物

試薬・触媒・溶媒 1

HCID 22728543Water ethylacetate溶媒

反応条件

温度
0 °C

実験手順

The compound obtained in Step E (20 mmol) is dissolved in a mixture of water/ethyl acetate (25 ml/75 ml) cooled to 0° C. Potassium carbonate (60 mmol) is added, and then acetyl chloride (26 mmol) is added dropwise to the reaction mixture. The mixture is stirred vigorously for 30 minutes at ambient temperature. The two phases are separated and the organic phase is washed with 0.1M aqueous hydrochloric acid solution and then with water. After drying over magnesium sulphate, the organic phase is evaporated under reduced pressure. The residue obtained is recrystallised from acetonitrile to yield the title product in the form of a white solid.

後処理

  1. customThe two phases are separated
  2. washthe organic phase is washed with 0.1M aqueous hydrochloric acid solution
  3. dry with materialAfter drying over magnesium sulphate
  4. customthe organic phase is evaporated under reduced pressure
  5. customThe residue obtained
  6. customis recrystallised from acetonitrile

出典と根拠

ORDレコード
ord-f2bc9330ad344068a5eecf2f38f2ba1d
出典データセット
uspto-grants-2011_05
特許番号
US07947852B2

反応ノート

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