4-Nitrophenyl morpholin-4-ylcarbamate → HCID 23513714、化合物

HRID 353435ノート

反応式

HRID 353435 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4](=[O:24])[CH:5]([C:12](=[O:23])[C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH2:21][Cl:22])=[CH:15][CH:14]=1)[C:6]2=[O:11].[N+](C1C=CC([O:34][C:35](=O)[NH:36][N:37]2[CH2:42][CH2:41][O:40][CH2:39][CH2:38]2)=CC=1)([O-])=O>CC#N.CN(C)C1C=CN=CC=1>[Cl:22][CH2:21][CH2:20][O:19][C:16]1[CH:17]=[CH:18][C:13]([C:12]([CH:5]2[C:4](=[O:24])[C:3]3[C:7](=[CH:8][CH:9]=[CH:10][C:2]=3[NH:1][C:35]([NH:36][N:37]3[CH2:42][CH2:41][O:40][CH2:39][CH2:38]3)=[O:34])[C:6]2=[O:11])=[O:23])=[CH:14][CH:15]=1

参加物

5

反応物 2

HCID 207362844-Nitrophenyl morpholin-4-ylcarbamateHCID 23513707HCID 23513707、化合物

生成物 1

HCID 23513714HCID 23513714、化合物収率 82%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 4-amino-2-[4-(2-chloroethoxy)benzoyl]indan-1,3-dione (36 g, 105 mmol) in CH3CN (600 mL) was added morpholin-4-ylcarbamic acid 4-nitrophenyl ester (40 g, 120 mmol) followed by 4-dimethylaminopyridine (640 mg, 5.2 mmol). The reaction was heated at reflux for 4 hours then cooled to room temp. and stirred overnight. The bright yellow solid is collected by filtration, rinsed with Et2O and dried under vacuum to give the desired semicarbazide (40.5 g, 82% yield).

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 4 hours
  3. temperaturethen cooled to room temp.
  4. filtrationThe bright yellow solid is collected by filtration
  5. washrinsed with Et2O
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-44876ec5d0b347e1b550d787396a8a34
出典データセット
uspto-grants-2004_06
特許番号
US06753329B2

反応ノート

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