Hydrochloric Acid → HCID 66647628、化合物

HRID 860820ノート

反応式

HRID 860820 の反応式
[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

参加物

12

反応物 7

HCID 313Hydrochloric Acid4 回HCID 6422Trifluoroacetic acid3 回HCID 21863450Trifluoroacetic acid methylene chlorideHCID 67908624HCID 67908624、化合物HCID 70166724HCID 70166724、化合物HCID 71777668Sulfuric acid, mixt. with nitric acidHCID 86601405HCID 86601405、化合物

生成物 1

HCID 66647628HCID 66647628、化合物

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 3776Isopropanol溶媒2 回HCID 6344Dichloromethane溶媒2 回HCID 8028Tetrahydrofuran溶媒3 回

実験手順

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.

後処理

  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.)

出典と根拠

ORDレコード
ord-0a2f012a0c8243b1a57d4a91d455005c
出典データセット
uspto-grants-2006_12
特許番号
US07153960B2

反応ノート

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