Hydrochloric Acid → HCID 22326703, 화합물

HRID 916633노트

반응식

HRID 916633 반응식
C([N:4]1[C:12]2[C:7](=[C:8]([O:13][CH2:14][CH2:15][Cl:16])[CH:9]=[CH:10][CH:11]=2)[CH:6]=[N:5]1)(=O)C.Cl>CO>[Cl:16][CH2:15][CH2:14][O:13][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[C:7]=1[CH:6]=[N:5][NH:4]2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22350151HCID 22350151, 화합물

생성물 1

HCID 22326703HCID 22326703, 화합물수율 96.9%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
65 °C

실험 절차

A stirred solution of 1-acetyl-4-(2-chloroethoxy)-indazole (1.50 g, 6.3 mmol) in methanol is treated with hydrochloric acid (6.3 ml, 1.0 M HCl in Et2O, 6.3 mmol) at room temperature, heated at 65° C. under nitrogen for 18 hr, cooled to room temperature and concentrated in vacuo. The resultant residue is neutralized with 1 N NaOH (6.0 ml) and diluted with H2O and ethyl acetate. The phases are separated and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with water and saturated NaCl, dried over Na2SO4 and concentrated in vacuo to afford the title product (1.2 g) as a yellow solid, identified by NMR and mass spectral analyses.

후처리

  1. temperaturecooled to room temperature
  2. concentrationconcentrated in vacuo
  3. additiondiluted with H2O and ethyl acetate
  4. customThe phases are separated
  5. extractionthe aqueous phase is extracted with ethyl acetate
  6. washThe combined organic phases are washed with water and saturated NaCl
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b3c126df56ce49b0a2428b32c8fefff9
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07271180B2

반응 노트

불러오는 중…