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 465907노트

반응식

HRID 465907 반응식
[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

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 682631,1'-CarbonyldiimidazoleHCID 13961228HCID 13961228, 화합물

생성물 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)-수율 39.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-79a966db9c0f4644948fadd626236327
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155103

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