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7-Benzenesulfonyl-4-(1-benzyl-pyrrolidin-3-yl)-3,4-dihydro-2H-benzo[1,4]oxazine → 7-benzenesulfonyl-4-pyrrolidin-3-yl-3,4-dihydro-2H-benzo[1,4]oxazine

HRID 2224082
ノート
印刷プレビュー

反応式

HRID 2224082 の反応式
[C:1]1([S:7]([C:10]2[CH:31]=[CH:30][C:13]3[N:14]([CH:18]4[CH2:22][CH2:21][N:20](CC5C=CC=CC=5)[CH2:19]4)[CH2:15][CH2:16][O:17][C:12]=3[CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(O)C.[Pd].C(O)(=O)C>[C:1]1([S:7]([C:10]2[CH:31]=[CH:30][C:13]3[N:14]([CH:18]4[CH2:22][CH2:21][NH:20][CH2:19]4)[CH2:15][CH2:16][O:17][C:12]=3[CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 586415207-Benzenesulfonyl-4-(1-benzyl-pyrrolidin-3-yl)-3,4-dihydro-2H-benzo[1,4]oxazine

生成物 1

HCID 116098757-benzenesulfonyl-4-pyrrolidin-3-yl-3,4-dihydro-2H-benzo[1,4]oxazine収率 44.7%

試薬・触媒・溶媒 3

HCID 176Acetic Acid触媒HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

7-Benzenesulfonyl-4-(1-benzyl-pyrrolidin-3-yl)-3,4-dihydro-2H-benzo[1,4]oxazine (0.127 g, 0.292 mmol) was dissolved in 15 mL ethanol and this solution was added to a flask containing 35 mg of 5% palladium on charcoal, followed by 3 drops of glacial acetic acid. The system was purged with hydrogen gas and stirring was continued for 24 hours under 1 atm. of hydrogen gas. The reaction mixture was filtered through celite, the filtrate concentrated in vacuo, and the resulting solid purified by flash (6:0.4:0.04 of CH2Cl2:MeOH:NH4OH) to give 45 mg of 7-benzenesulfonyl-4-pyrrolidin-3-yl-3,4-dihydro-2H-benzo[1,4]oxazine as free base. This solid was dissolved in 1 mL methanol and combined with 0.5 mL of 2N ethanolic hydrogen chloride and the resulting solution is concentrated in vacuo and subjected to a vacuum of 0.3 Torr for 2 hours to give a foam which was triturated twice with 50 mL ethyl ether to give, after drying under reduced pressure, 25 mg (0.07 mmol, 25%) of 7-benzenesulfonyl-4-pyrrolidin-3-yl-3,4-dihydro-2H-benzo[1,4]oxazine hydrochloride as a tan solid. MS: 345 (M+H)+, mp: 122.8-127.6° C.

後処理

  1. additionthis solution was added to a flask
  2. customThe system was purged with hydrogen gas
  3. filtrationThe reaction mixture was filtered through celite
  4. concentrationthe filtrate concentrated in vacuo
  5. customthe resulting solid purified by flash (6:0.4:0.04 of CH2Cl2:MeOH:NH4OH)

出典と根拠

ORDレコード
ord-64ac33af5d1642c990f0b6f3b2f15b4a
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07378415B2

反応ノート

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