Ammonia → 4-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzamide

HRID 515483노트

반응식

HRID 515483 반응식
[C:1]1([C@H:7]([N:9]2[CH2:15][CH2:14][CH:13]([C:16]3[CH:24]=[CH:23][C:19]([C:20](O)=[O:21])=[CH:18][CH:17]=3)[O:12][CH2:11][CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.N.[Cl-].COC1N=C(OC)N=C([N+]2(C)CCOCC2)[N:32]=1>CN(C)C=O.O>[C:1]1([C@H:7]([N:9]2[CH2:15][CH2:14][CH:13]([C:16]3[CH:24]=[CH:23][C:19]([C:20]([NH2:32])=[O:21])=[CH:18][CH:17]=3)[O:12][CH2:11][CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 887MethanolHCID 27340594-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chlorideHCID 672831054-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzoic acid

생성물 1

HCID 672820504-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzamide

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzoic acid (diastereomer type A) (0.96 g, 2.9 mmol) and 7 mol/L methanol solution of ammonia (2 mL, 14 mmol) in N,N-dimethylformamide (10 mL) was added 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (1.25 g, 4.5 mmol) at room temperature and the mixture was stirred for one day. The reaction mixture was poured into water. The resulting white solid material was collected by filtration and dried under reduced pressure at 50° C. for 5 hours to yield 4-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzamide (diastereomer type A) (0.58 g, 1.78 mmol, 61%).

후처리

  1. filtrationThe resulting white solid material was collected by filtration
  2. customdried under reduced pressure at 50° C. for 5 hours

출처 및 근거

ORD 기록
ord-a77b7ebc592a4110b3d193610203c98a
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108957B2

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