Hydrochloric Acid → HCID 136082911, 화합물

HRID 1788000노트

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HRID 1788000 반응식
C[O:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([N:12]3[C:20](=[O:21])[C:19]4[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:13]3=[O:22])=[N:8][NH:9]2)=[CH:5][CH:4]=1.Cl.N1C=CC=CC=1.Cl>C(OCC)(=O)C>[OH:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([N:12]3[C:20](=[O:21])[C:19]4[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:13]3=[O:22])=[N:8][NH:9]2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10176127Pyridinium chlorideHCID 66749847HCID 66749847, 화합물

생성물 1

HCID 136082911HCID 136082911, 화합물수율 69%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
200 °C

실험 절차

A mixture of 24.2 g (82.5 mmol) of 2-({6-methoxy}-1H-indazol-3-yl)-1H-isoindole-1,3(2H)-dione and 73.4 g (0.635 mol) of piridine hydrochloride was heated at 200° C. for 4 hours. The resulting brown solution was cooled to 140° C. and slowly poured in a well stirred mixture of 250 ml of 0.2 N HCl and 350 ml of ethyl acetate. The organic layer was separated and the aqueous layer was salted (45 g of NaCl) and extracted twice with 350 ml of ethyl acetate. Organic extracts were dried over sodium sulfate and concentrated under vacuum to small volume. The precipitate was filtered off and dried: 15.89 g of product as yellow solid were obtained. Yield=68.9%. mp=265-270° C. dec.

후처리

  1. temperatureThe resulting brown solution was cooled to 140° C.
  2. additionslowly poured in a well
  3. customThe organic layer was separated
  4. extractionextracted twice with 350 ml of ethyl acetate
  5. dry with materialOrganic extracts were dried over sodium sulfate
  6. concentrationconcentrated under vacuum to small volume
  7. filtrationThe precipitate was filtered off
  8. customdried

출처 및 근거

ORD 기록
ord-f12aead606f24a7b964da767f75a6aec
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07511136B2

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