Water → HCID 46245273, 화합물

HRID 1846575노트

반응식

HRID 1846575 반응식
Cl.[NH:2]1[C:7]2[N:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2([CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[O:4][C:3]1=[O:17].Cl[C:19]1[N:24]=[C:23]([CH3:25])[N:22]=[C:21]([O:26][C:27]2[CH:36]=[C:35]([CH3:37])[C:30]3[NH:31][C:32](=[O:34])[O:33][C:29]=3[CH:28]=2)[CH:20]=1.CCN(C(C)C)C(C)C.O>CN(C=O)C.C(Cl)Cl>[CH3:37][C:35]1[C:30]2[NH:31][C:32](=[O:34])[O:33][C:29]=2[CH:28]=[C:27]([O:26][C:21]2[CH:20]=[C:19]([N:14]3[CH2:13][CH2:12][C:5]4([O:4][C:3](=[O:17])[NH:2][C:7]5[N:8]=[CH:9][CH:10]=[CH:11][C:6]4=5)[CH2:16][CH2:15]3)[N:24]=[C:23]([CH3:25])[N:22]=2)[CH:36]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 81531Diisopropylethylamine2회HCID 66687106Spiro[piperidine-4,4'-pyrido[2,3-d][1,3]oxazin]-2'(1'H)-one hydrochloride2회HCID 86663906HCID 86663906, 화합물

생성물 1

HCID 46245273HCID 46245273, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
60 °C

실험 절차

90 mg (0.35 mmol) spiro[piperidin-4,4′-pyrido[2,3-d][1,3]oxazin]-2′(1′H)-one hydrochloride, 90 mg (0.31 mmol) 6-(6-chloro-2-methylpyrimidin-4-yloxy)-4-methylbenzo[d]oxazol-2(3H)-one and 200 μL (1.16 mmol) DIPEA in 1.5 mL DMF were stirred overnight at RT. Another 90 mg (0.35 mmol) spiro[piperidin-4,4′-pyrido[2,3-d][1,3]oxazin]-2′(1′H)-one hydrochloride and 200 μL (1.16 mmol) DIPEA were added and the mixture was stirred for 8 h at 60° C. The reaction mixture was mixed with water and stirred overnight. Then DCM was added and the mixture was stirred for a further 30 min. DCM was removed and the aqueous phase was suction filtered. The precipitate was washed with EtOH and dried.

후처리

  1. stirringstirred overnight
  2. stirringthe mixture was stirred for a further 30 min
  3. customDCM was removed
  4. washThe precipitate was washed with EtOH
  5. customdried

출처 및 근거

ORD 기록
ord-03721f69cde5460caca51273d8fa94d1
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952014B2

반응 노트

불러오는 중…