Tributylamine → HCID 178432402、化合物

HRID 1986636ノート

反応式

HRID 1986636 の反応式
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.[CH:7]1([CH:12]([C:18](=O)[CH3:19])[C:13](OCC)=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8]1.C(N(CCCC)CCCC)CCC>[OH-].[Na+]>[CH3:19][C:18]1[C:12]([CH:7]2[CH2:11][CH2:10][CH2:9][CH2:8]2)=[C:13]([OH:14])[N:3]2[N:4]=[CH:5][N:6]=[C:2]2[N:1]=1

参加物

5

反応物 3

HCID 7622TributylamineHCID 17750296Ethyl 2-cyclopentyl-3-oxobutanoateHCID 178418311HCID 178418311、化合物

生成物 1

HCID 178432402HCID 178432402、化合物収率 52.3%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
180 °C

実験手順

A mixture of 3-amino-1,2,4-triazole (14 g), ethyl 2-cyclopentyl-3-oxobutanoate (0.17 mol, Ex. 1) and tributylamine (50 ml) was heated at 180° C. for 6 hours. The reaction mixture was cooled to about 70° C., and aqueous NaOH solution (21 g in 200 ml of H2O) was then added and the solution was stirred for another 30 min. Following phase separation and extraction with diethyl ether, the aqueous phase was acidified with conc. HCl solution. The precipitate gave 19 g of the title compound.

後処理

  1. temperatureThe reaction mixture was cooled to about 70° C.
  2. customFollowing phase separation and extraction with diethyl ether

出典と根拠

ORDレコード
ord-57d71b38b94e4789b7f567a5272e2cb5
出典データセット
uspto-grants-2009_06
特許番号
US07550471B2

反応ノート

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