Hydrochloric Acid → HCID 66647628, 화합물

HRID 860820노트

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HRID 860820 반응식
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.[NH:6]1C=C[CH:9]=[CH:8][C:7]1=O.FC(F)(F)C(O)=[O:16].[N+]([O-])(O)=O.S(=O)(=O)(O)O.Cl.FC(F)(F)C(O)=O.C(Cl)Cl.Cl.C(O)(C)C.C1COCC1.Cl.O.C1COCC1>C(O)(C)C.C(Cl)Cl.C1COCC1.O>[N:1]1[C:5]2[CH:9]=[CH:8][CH:7]=[N:6][C:4]=2[C:3](=[O:16])[N:2]=1

참가 물질

12

반응물 7

HCID 313Hydrochloric Acid4회HCID 6422Trifluoroacetic acid3회HCID 21863450Trifluoroacetic acid methylene chlorideHCID 67908624HCID 67908624, 화합물HCID 70166724HCID 70166724, 화합물HCID 71777668Sulfuric acid, mixt. with nitric acidHCID 86601405HCID 86601405, 화합물

생성물 1

HCID 66647628HCID 66647628, 화합물

시약·촉매·용매 4

HCID 962Water용매HCID 3776Isopropanol용매2회HCID 6344Dichloromethane용매2회HCID 8028Tetrahydrofuran용매3회

실험 절차

Fused pyrazoline (III) can be converted to its corresponding pyrazole-pyridinone (IV) by treatment with an acid. This deamination reaction is preferably performed in the presence of a strong acid (e.g., trifluoroacetic acid (TFA), sulfuric acid nitric acid, and hydrochloric acid (HCl)). An aprotic solvent may be used (e.g., CH2Cl2 or THF). As one of ordinary skill in the art recognizes, some acids are usually available in the presence of a second solvent. For example, 6N HCl can be available in isopropyl alcohol (IPA). 2N HCl can be available as an aqueous solution. Thus, the second solvent, if present, will depend on the acid used. Preferably, the second solvent is isopropyl alcohol or water. The reaction can be conducted from about 5° C. to reflux of the solvent. Preferably, when TFA, either neat or in CH2Cl2, is used, the reaction is conducted at a temperature of from 5° C. to room temperature (approximately 25° C.). Preferably, when HCl (e.g., 2N or 6N) is used, the reaction solvent is THF and the reaction is conducted at about the reflux temperature of THF. Preferred acids or acid solvent combinations are: TFA (neat), TFA/CH2Cl2, 6N HCl/isopropyl alcohol/THF, and 2N HCl/water/THF.

후처리

  1. customThis deamination reaction
  2. customThe reaction
  3. customcan be conducted from about 5° C.
  4. temperatureto reflux of the solvent
  5. customis conducted at a temperature of from 5° C. to room temperature (approximately 25° C.)

출처 및 근거

ORD 기록
ord-0a2f012a0c8243b1a57d4a91d455005c
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07153960B2

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