Acetic Acid → 6-(tert-butyl)phthalazin-1(2H)-one

HRID 600367노트

반응식

HRID 600367 반응식
[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=O)[O:9][CH:8]2OCC)([CH3:4])([CH3:3])[CH3:2].O.[NH2:19][NH2:20].C(O)(=O)C>O>[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:9])[NH:20][N:19]=[CH:8]2)([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 580162095-tert-Butyl-3-ethoxy-3H-isobenzofuran-1-one

생성물 1

HCID 576339336-(tert-butyl)phthalazin-1(2H)-one수율 92.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2.9 g (12 mmol) of 5-tert-butyl-3-ethoxy-3H-isobenzofuran-1-one was weighed into a 50 mL round bottom flask fitted with a stir bar and cap. Added 10 mL (130 mmol) of hydrazine monohydrate. Added 15 mL of glacial acetic acid. Stirred at 100° overnight. Poured the reaction mixture into 200 mL of stirred water. Collected the solids by filtration and washed with water. Dried under high vacuum to obtain 2.24 g of the title compound as an off-white solid. MS (ESI) 203 (M+H)+.

후처리

  1. customfitted with a stir bar
  2. customcap
  3. customCollected the solids
  4. filtrationby filtration
  5. washwashed with water
  6. customDried under high vacuum

출처 및 근거

ORD 기록
ord-cf94e078f67449099c865a142bbe3ffa
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902194B2

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