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N-methyl-2-pyrrolidone → HCID 66940819、化合物

HRID 2192467
ノート
印刷プレビュー

反応式

HRID 2192467 の反応式
Cl[C:2]1[C:11]2[C:6](=[C:7]([C:12]3[N:16]=[C:15]([C:17]4[CH:22]=[CH:21][C:20]([O:23][CH:24]([CH3:26])[CH3:25])=[C:19]([Cl:27])[CH:18]=4)[O:14][N:13]=3)[CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.C(N(C(C)C)CC)(C)C.[NH2:37][CH2:38][CH2:39][C:40]([O:42][C:43]([CH3:46])([CH3:45])[CH3:44])=[O:41].CN1CCCC1=O>CO>[Cl:27][C:19]1[CH:18]=[C:17]([C:15]2[O:14][N:13]=[C:12]([C:7]3[CH:8]=[CH:9][CH:10]=[C:11]4[C:6]=3[CH:5]=[CH:4][N:3]=[C:2]4[NH:37][CH2:38][CH2:39][C:40]([O:42][C:43]([CH3:46])([CH3:45])[CH3:44])=[O:41])[N:16]=2)[CH:22]=[CH:21][C:20]=1[O:23][CH:24]([CH3:26])[CH3:25]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 13387N-methyl-2-pyrrolidoneHCID 81531DiisopropylethylamineHCID 4192171tert-Butyl 3-aminopropanoateHCID 58149900HCID 58149900、化合物

生成物 1

HCID 66940819HCID 66940819、化合物収率 14.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
180 °C

実験手順

1-Chloro-5-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)isoquinoline (D7; 200 mg, 0.5 mmol), di-isopropylethylamine (0.873 ml, 1.0 mmol) and 1,1-dimethylethyl β-alaninate (726 mg, 5 mmol; available e.g. from Novabiochem) were placed into a 20 ml microwave vial, and N-methyl-2-pyrrolidinone (NMP, 8 ml) was added. The mixture was heated under microwave irradiation at 180° C. for one hour, diluted with methanol and chromatographed over an SCX cation exchange column (Biotage), which was washed with methanol and dichloromethane and eluted with methanolic ammonia. Washings and eluate from the SCX column were re-combined and evaporated in vacuo until only NMP remained. Water (20 ml) was added to the reaction mixture and a solid precipitate formed. The precipitate was collected by filtration and azeotroped twice with toluene. The solid was dissolved in dichloromethane (5 ml) and chromatographed on a silica column, eluting with dichloromethane to yield the title compound (38 mg) as a pale yellow solid.

後処理

  1. customchromatographed over an SCX cation exchange column (Biotage), which
  2. washwas washed with methanol and dichloromethane
  3. washeluted with methanolic ammonia
  4. customevaporated in vacuo until only NMP
  5. additionWater (20 ml) was added to the reaction mixture
  6. customa solid precipitate formed
  7. filtrationThe precipitate was collected by filtration
  8. customazeotroped twice with toluene
  9. dissolutionThe solid was dissolved in dichloromethane (5 ml)
  10. customchromatographed on a silica column
  11. washeluting with dichloromethane

出典と根拠

ORDレコード
ord-8b477940815c447fb8d6f493668e23b2
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329730B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート