Morpholine → Morpholine, 4-((4-(2-chlorophenyl)-9-methyl-6H-thieno(3,2-f)(1,2,4)triazolo(4,3-a)(1,4)diazepin-2-yl)acetyl)-

HRID 465907ノート

反応式

HRID 465907 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([CH2:18][C:19]([OH:21])=O)[S:17][C:13]=2[N:12]2[C:22]([CH3:25])=[N:23][N:24]=[C:11]2[CH2:10][N:9]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.[NH:38]1[CH2:43][CH2:42][O:41][CH2:40][CH2:39]1>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([CH2:18][C:19]([N:38]3[CH2:43][CH2:42][O:41][CH2:40][CH2:39]3)=[O:21])[S:17][C:13]=2[N:12]2[C:22]([CH3:25])=[N:23][N:24]=[C:11]2[CH2:10][N:9]=1

参加物

5

反応物 3

HCID 8083MorpholineHCID 682631,1'-CarbonyldiimidazoleHCID 13961228HCID 13961228、化合物

生成物 1

HCID 3087284Morpholine, 4-((4-(2-chlorophenyl)-9-methyl-6H-thieno(3,2-f)(1,2,4)triazolo(4,3-a)(1,4)diazepin-2-yl)acetyl)-収率 39.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Here, [4-(2-chlorophenyl)-9-methyl-6H-thieno[3,2-f][1,2,4]-triazolo[4,3-a][1,4]diazepin-2-yl]-methane carboxylic acid (20 g, 0.054 mol), tetrahydrofuran (500 ml) and 1,1'-carbonyldiimidazole (10 g) are stirred for 1 hour at ambient temperature and the solution, now clear, is mixed with morpholine (0.06 mol, 5.2 g). After stirring overnight at ambient temperature, evaporation, taking up in methylene chloride, washing with sodium bicarbonate solution and filtering through a column of SiO2, the title compound (9.4 g), m.p. 143°-144° C., is obtained by recrystallization from ethyl acetate.

後処理

  1. customevaporation
  2. washwashing with sodium bicarbonate solution
  3. filtrationfiltering through a column of SiO2

出典と根拠

ORDレコード
ord-79a966db9c0f4644948fadd626236327
出典データセット
uspto-grants-1992_10
特許番号
US05155103

反応ノート

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