1-Hydroxybenzotriazole → HCID 178482473、化合物

HRID 1620506ノート

反応式

HRID 1620506 の反応式
[CH3:1][C:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:11]([OH:13])=O.ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C.Cl.Cl.[CH3:38][NH:39][C:40]1=[N:41][C:42](=[O:52])[S:43]/[C:44]/1=[CH:45]\[CH:46]1[CH2:51][CH2:50][NH:49][CH2:48][CH2:47]1>CN(C)C=O.O.C(N(CC)CC)C>[CH3:38][NH:39][C:40]1=[N:41][C:42](=[O:52])[S:43]/[C:44]/1=[CH:45]\[CH:46]1[CH2:51][CH2:50][N:49]([C:11]([C:3]2[O:4][C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=3[C:2]=2[CH3:1])=[O:13])[CH2:48][CH2:47]1

参加物

8

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 6005913-Methyl-1-benzofuran-2-carboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 178482469HCID 178482469、化合物

生成物 1

HCID 178482473HCID 178482473、化合物収率 50.4%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

To a solution of 3-methyl-1-benzofuran-2-carboxylic acid (19.4 mg) in N,N-dimethylformamide (1 mL) were added 1-hydroxybenzotriazole (16.2 mg) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (23 mg), and the mixture was stirred at 0° C. for 5 min. To the reaction mixture were added triethylamine (0.28 mL) and (5Z)-4-(methylamino)-5-(piperidin-4-ylmethylidene)-1,3-thiazol-2(5H)-one dihydrochloride (29.8 mg), and the mixture was further stirred at room temperature for 5 hr. Water was added to the reaction mixture, and the precipitate was collected by filtration, and washed with water and diisopropyl ether to give the title compound (19.3 mg).

後処理

  1. stirringthe mixture was further stirred at room temperature for 5 hr
  2. filtrationthe precipitate was collected by filtration
  3. washwashed with water and diisopropyl ether

出典と根拠

ORDレコード
ord-f7f2c43d813340dab9155750bcee77d6
出典データセット
uspto-grants-2014_07
特許番号
US08772277B2

反応ノート

読み込み中…