Water → 1-Iodo-2-cyano-4-propoxy-benzene

HRID 330837노트

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HRID 330837 반응식
O=S(Cl)Cl.[I:5][C:6]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][CH3:18])=[CH:11][C:7]=1[C:8]([NH2:10])=O.O>CN(C=O)C>[I:5][C:6]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][CH3:18])=[CH:11][C:7]=1[C:8]#[N:10]

참가 물질

5

반응물 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 666113302-Iodo-5-propoxy-benzamide

생성물 1

HCID 666142061-Iodo-2-cyano-4-propoxy-benzene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
115 °C

실험 절차

1.67 mL (22.9 mmol) SOCl2 are added to 1.40 g (4.59 mmol) 2-iodo-5-propoxy-benzamide (XXIX.1) in 40 mL DMF. The mixture is stirred at 115° C. for 1 h. After that time, water is added and the mixture is extracted with EtOAc (3×). The combined organic layers are washed with water and brine, dried over sodium sulphate and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, heptane/EtOAc 100/0→60/40).

후처리

  1. extractionthe mixture is extracted with EtOAc (3×)
  2. washThe combined organic layers are washed with water and brine
  3. dry with materialdried over sodium sulphate
  4. customthe solvent is removed in vacuo
  5. customThe crude product is purified by column chromatography (silica gel, heptane/EtOAc 100/0→60/40)

출처 및 근거

ORD 기록
ord-a0b5b6a789ff4f9f948b06fda70b774f
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877754B2

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