Hydrochloric Acid → Methyl 4-(2-aminoethoxy)benzoate

HRID 583674노트

반응식

HRID 583674 반응식
C1(=O)[N:5]([CH2:6][CH2:7][O:8][C:9]2[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=2)C(=O)C2=CC=CC=C12.NN.Cl>CO>[NH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 7679064Methyl 4-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)benzoate

생성물 1

HCID 14097616Methyl 4-(2-aminoethoxy)benzoate

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

19-2 (1.59 g, 4.89 mmol) was suspended in 25 mL MeOH. Upon addition of hydrazine (2.0 mL, 64 mmol) the reaction became homogeneous. After 20 h a heavy precipitate had formed. The pH was adjusted to 1 by addition of 6N HCl, MeOH evaporated, and the solid suspended in 1N HCl. After filtering through Celite, the filtrate was washed with CH2Cl2, the pH was adjusted to 12 with 6N NaOH. The aqueous layer was extracted with fresh CH2Cl2. This organic phase was dried (Na2SO4) and concentrated providing 19-3 as a white solid.

후처리

  1. customAfter 20 h a heavy precipitate had formed
  2. customevaporated
  3. filtrationAfter filtering through Celite
  4. washthe filtrate was washed with CH2Cl2
  5. extractionThe aqueous layer was extracted with fresh CH2Cl2
  6. dry with materialThis organic phase was dried (Na2SO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ec48a48efae34717823a739ab5194fd2
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929120

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