Acetic Acid → HCID 23048269、化合物

HRID 2107347ノート

反応式

HRID 2107347 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 conc. 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 equeous 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 dehydrating by azeotropic distillation or in the presence of molecular sieve to give the hexahydroindazol-3-one (II).

後処理

  1. distillationwhile dehydrating by azeotropic distillation or in the presence of molecular sieve

出典と根拠

ORDレコード
ord-92168e33961348d4aafe0b04763ad70b
出典データセット
uspto-grants-1990_06
特許番号
US04933480

反応ノート

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