1,2-Dichloroethane → HCID 57448175, 화합물

HRID 1667584노트

반응식

HRID 1667584 반응식
[CH:1]1([S:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8](O)=[O:9])[CH2:4][CH2:3][CH2:2]1.C1C=CC2N(O)N=[N:21]C=2C=1.O.C(Cl)CCl.[OH-].[NH4+]>CN(C=O)C.C(OCC)(=O)C.C1COCC1>[CH:1]1([S:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8]([NH2:21])=[O:9])[CH2:4][CH2:3][CH2:2]1

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 962WaterHCID 14923Ammonium HydroxideHCID 757711-HydroxybenzotriazoleHCID 57448174HCID 57448174, 화합물

생성물 1

HCID 57448175HCID 57448175, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 21939870Tetrahydrofuran ethyl acetate용매

실험 절차

To 2B (6.30 g, 26.2 mmol) in DMF (52.5 mL) was added HOBT.H2O (4.9 g, 32.0 mmol) and EDC (5.98 g, 31.3 mmol). After stirring 1 h at rt, the reaction was cooled to 0° C. and 25% ammonium hydroxide was added. The reaction was stirred for 1.5 h and was then diluted with ethyl acetate/THF and washed with 1N HCl (2×) and 1 N NaOH (2×). The aqueous layer was back-extracted with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), filtered and concentrated to provide 2C (5 g) as a yellow solid. LC-MS: 240.08 (M+H)+.

후처리

  1. temperaturethe reaction was cooled to 0° C.
  2. stirringThe reaction was stirred for 1.5 h
  3. washwashed with 1N HCl (2×) and 1 N NaOH (2×)
  4. extractionThe aqueous layer was back-extracted with ethyl acetate
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-76e8462bc4f44d2185b56d242a764653
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044242B2

반응 노트

불러오는 중…