Water → HCID 46245273、化合物

HRID 1846575ノート

反応式

HRID 1846575 の反応式
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

参加物

7

反応物 4

HCID 962WaterHCID 81531Diisopropylethylamine2 回HCID 66687106Spiro[piperidine-4,4'-pyrido[2,3-d][1,3]oxazin]-2'(1'H)-one hydrochloride2 回HCID 86663906HCID 86663906、化合物

生成物 1

HCID 46245273HCID 46245273、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-03721f69cde5460caca51273d8fa94d1
出典データセット
uspto-grants-2015_02
特許番号
US08952014B2

反応ノート

読み込み中…