Triethylamine → [2-Amino-5-(2-methyl-1,3-dioxolan-2-yl)phenyl](phenyl)methanone

HRID 1380008노트

반응식

HRID 1380008 반응식
[CH3:1][C:2]1([C:7]2[CH:8]=[CH:9][C:10]3[C:11]([CH:21]=2)=[C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[O:13][N:14]=3)[O:6][CH2:5][CH2:4][O:3]1.C(N(CC)CC)C>[Pd].O1CCCC1>[NH2:14][C:10]1[CH:9]=[CH:8][C:7]([C:2]2([CH3:1])[O:3][CH2:4][CH2:5][O:6]2)=[CH:21][C:11]=1[C:12]([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)=[O:13]

참가 물질

5

반응물 2

HCID 8471TriethylamineHCID 6497105-(2-Methyl-1,3-dioxolan-2-yl)-3-phenyl-2,1-benzoxazole

생성물 1

HCID 21828105[2-Amino-5-(2-methyl-1,3-dioxolan-2-yl)phenyl](phenyl)methanone수율 89.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

5-(2-Methyl-1,3-dioxolan-2yl)-3-phenyl-2,1-benzisoxazole (1.50 g, 5.3 m mol), triethyl amine (0.3 ml) and 5% palladium on carbon (0.15 g) were combined in dry tetrahydrofuran (13 ml). The apparatus wa flushed with nitrogen and then hydrogen. A static hydrogen atmosphere was maintained (1 atm.) and the progress of the reaction followed by gas chromatography. The starting material and product have retention times of 11.15 and 11.33 min. respectively. When conversion was complete, the mixture was filtered through a pad of Celite to yield a clear yellow solution. Evaporation of the solution yielded a yellow solid (1.35 g) of mp. 108°-111° C.

후처리

  1. customThe apparatus wa flushed with nitrogen
  2. temperatureA static hydrogen atmosphere was maintained (1 atm.)
  3. customretention times of 11.15 and 11.33 min.
  4. filtrationthe mixture was filtered through a pad of Celite
  5. customto yield a clear yellow solution
  6. customEvaporation of the solution

출처 및 근거

ORD 기록
ord-7916e66951aa4045a2a503851fc4f45d
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579679

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