Acetic Acid → HCID 23048269、化合物

HRID 580247ノート

反応式

HRID 580247 の反応式
[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

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1140TolueneHCID 129772811HCID 129772811、化合物

生成物 1

HCID 23048269HCID 23048269、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

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).

後処理

  1. distillationby azeotropic distillation

出典と根拠

ORDレコード
ord-4ca7f12345c64887b30090ace301af26
出典データセット
uspto-grants-1988_06
特許番号
US04752325

反応ノート

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