Water → 3-Chloropropyl (3-hydroxymethylphenyl)carbamate

HRID 655310

반응식

HRID 655310 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 595647253-Chloropropyl (3-hydroxymethylphenyl)carbamate

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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;

후처리

  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

출처 및 근거

ORD 기록
ord-5d8c0b52738e4576a6b5110ee3e74510
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071593B2

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