Water → 3-Chloropropyl (3-hydroxymethylphenyl)carbamate

HRID 655310

反応式

HRID 655310 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6].C(=O)([O-])[O-].[Na+].[Na+].Cl[C:17]([O:19][CH2:20][CH2:21][CH2:22][Cl:23])=[O:18].O>CC(C)=O>[OH:6][CH2:5][C:4]1[CH:3]=[C:2]([NH:1][C:17](=[O:18])[O:19][CH2:20][CH2:21][CH2:22][Cl:23])[CH:9]=[CH:8][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 69399Carbonochloridic acid, 3-chloropropyl esterHCID 802933-Aminobenzyl alcohol

生成物 1

HCID 595647253-Chloropropyl (3-hydroxymethylphenyl)carbamate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

3.7 g (30 mmol) of 3-aminobenzyl alcohol are dissolved in 50 ml of acetone, and 3.2 g (30 mmol) of sodium carbonate are added. 5.7 g (36 mmol) of 3-chloropropyl chloroformate are metered into this suspension at 25° C. The reaction mixture is stirred at room temperature for a further 18 h. Water is added to the reaction mixture for hydrolysis, and the solid is subsequently filtered off. The solution is concentrated by distillation, during which the product deposits as an oil. The product phase is separated off. The aqueous phase is extracted with ethyl acetate. The organic phases are combined, washed with water and dried over sodium sulfate. The mixture is subsequently evaporated to dryness. The crude product is reacted further directly without further purification;

後処理

  1. customare metered into this suspension at 25° C
  2. filtrationthe solid is subsequently filtered off
  3. concentrationThe solution is concentrated by distillation, during which the product deposits as an oil
  4. customThe product phase is separated off
  5. extractionThe aqueous phase is extracted with ethyl acetate
  6. washwashed with water
  7. dry with materialdried over sodium sulfate
  8. customThe mixture is subsequently evaporated to dryness
  9. customThe crude product is reacted further directly without further purification

出典と根拠

ORDレコード
ord-5d8c0b52738e4576a6b5110ee3e74510
出典データセット
uspto-grants-2011_12
特許番号
US08071593B2

関連ノート

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