Triethylamine hydrofluoride → trans-N-(2-benzyloxycyclohexyl)-N'-(2-hydroxy-4-nitrophenyl)urea

HRID 368378노트

반응식

HRID 368378 반응식
[CH2:1]([O:8][C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C@H:10]1[NH:15][C:16]([NH:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][C:20]=1[O:28][Si](C(C)(C)C)(C)C)=[O:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.F.C(N(CC)CC)C>C(#N)C>[CH2:1]([O:8][C@@H:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C@H:10]1[NH:15][C:16]([NH:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][C:20]=1[OH:28])=[O:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 10290782Triethylamine hydrofluorideHCID 15485711trans-N-(2-Benzyloxycyclohexyl)-N'-(2-tert-butyldimethylsilyloxy-4-nitrophenyl) urea

생성물 1

HCID 15485712trans-N-(2-benzyloxycyclohexyl)-N'-(2-hydroxy-4-nitrophenyl)urea수율 95%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of trans-N-(2-Benzyloxycyclohexyl)-N'-(2-tert-butyldimethylsilyloxy-4-nitrophenyl) urea (100 mg, 0.2 mmol) in acetonitrile (2 mL), triethylamine hydrofluoride (0.1 mL, 0.6 mmol) was added. The reaction mixture was stirred at room temperature for 30 minutes. The reaction mixture was partitioned between ethyl acetate and water. The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure to give product (73 mg, 95%). EI-MS m/z 386 (M+H)+.

후처리

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-19e51050e09d4a3e9fac3f01f6720d08
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133319

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