Acetic Acid → HCID 23048269, 화합물

HRID 580247노트

반응식

HRID 580247 반응식
[NH2:1](=S)[NH2:2].[C:4]([OH:7])(=O)[CH3:5].[C:8]1(C)[CH:13]=[CH:12]C=[CH:10][CH:9]=1>C1(C)C(C)=CC=CC=1>[NH:1]1[C:10]2[CH:5]([CH2:12][CH2:13][CH2:8][CH:9]=2)[C:4](=[O:7])[NH:2]1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1140TolueneHCID 129772811HCID 129772811, 화합물

생성물 1

HCID 23048269HCID 23048269, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

The aminosulfide (IV) is then reacted with concentrated hydrochloric acid at a temperature of 0° to 40° C., followed by reacting the resultant hydrochloride with 1.0 to 1.5 equivalents of sodium nitrite at -10° to 5° C. to form the diazonium salt. The diazonium salt is reduced with 3.0 to 10 equivalents (in regard to the aminosulfide (IV)) of stannous chloride at 0° to -40° C. to obtain the hydrazine hydrochloride, which is neutralized with an aqueous alkaline solution (e.g. sodium hydroxide, potassium hydroxide, potassium carbonate) to obtain the hydrazine sulfide (V). The thus obtained hydrazine sulfide (V) is reacted with 1.0 to 1.2 equivalents of 2-alkoxycarbonylcyclohexanone in a solvent (e.g. acetic acid, toluene, xylene) at a temperature of 50° to 200° C. (preferably 80° to 150° C.) optionally while dehydration by azeotropic distillation or in the presence of molecular sieve is conducted to give the hexahydroindazol-3-one (II).

후처리

  1. distillationby azeotropic distillation

출처 및 근거

ORD 기록
ord-4ca7f12345c64887b30090ace301af26
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752325

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