4-Nitrophenyl morpholin-4-ylcarbamate → HCID 23513714, 화합물

HRID 1821450노트

반응식

HRID 1821450 반응식
[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

참가 물질

5

반응물 2

HCID 207362844-Nitrophenyl morpholin-4-ylcarbamateHCID 23513707HCID 23513707, 화합물

생성물 1

HCID 23513714HCID 23513714, 화합물수율 82%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-82d18d8bb6ec44dbb21c6af4963da08a
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07605175B2

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