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Acetyl chloride → HCID 67966825、化合物

HRID 527659
ノート
印刷プレビュー

反応式

HRID 527659 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH3:9])[C:3]=1[C:10]([OH:13])([CH3:12])[CH3:11].C(N(CC)CC)C.[C:21](Cl)(=[O:23])[CH3:22].[NH4+].[Cl-]>C(Cl)Cl>[OH:13][C:10]([C:3]1[C:4]([O:8][CH3:9])=[CH:5][CH:6]=[CH:7][C:2]=1[NH:1][C:21](=[O:23])[CH3:22])([CH3:11])[CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 67958514HCID 67958514、化合物2 回

生成物 1

HCID 67966825HCID 67966825、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

2-(2-Amino-6-methoxyphenyl)propan-2-ol (Intermediate 199, 500 mg, 2.76 mmol) was dissolved in DCM (10 mL) and triethylamine (0.770 ml, 5.52 mmol) was added. The solution was cooled to 0° C. and treated with acetyl chloride (0.2 ml, 2.76 mmol) in a drop wise fashion. At the end of the addition, complete conversion was reached. The mixture was treated with an aqueous saturated solution of NH4Cl, two phases were separated and the organic layer was washed with an aqueous saturated solution of NaHCO3 and brine, then dried over Na2SO4 and evaporated to dryness. The crude was purified by re-slurry in tert-butyl methyl ether isolating 490 mg of the title compound as white solid.

後処理

  1. additionAt the end of the addition, complete conversion
  2. customwere separated
  3. washthe organic layer was washed with an aqueous saturated solution of NaHCO3 and brine
  4. dry with materialdried over Na2SO4
  5. customevaporated to dryness
  6. customThe crude was purified by re-slurry in tert-butyl methyl ether isolating 490 mg of the title compound as white solid

出典と根拠

ORDレコード
ord-5301aa62c5f344e187fa6bfdc206ada3
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09346790B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート