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Triphenylphosphine → HCID 21963144、化合物

HRID 2211822
ノート
印刷プレビュー

反応式

HRID 2211822 の反応式
[OH:1][CH:2]1[CH2:6][CH2:5][N:4]([C:7]2[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][CH:8]=2)[C:3]1=[O:17].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=1[N:44]1[CH2:49][CH2:48][N:47]([C:50]([O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[O:51])[CH2:46][CH2:45]1.N(C([O-])=O)=NC([O-])=O>O1CCCC1>[C:53]([O:52][C:50]([N:47]1[CH2:48][CH2:49][N:44]([C:39]2[CH:40]=[CH:41][CH:42]=[CH:43][C:38]=2[O:1][CH:2]2[CH2:6][CH2:5][N:4]([C:7]3[CH:8]=[CH:9][C:10]([C:13]([F:14])([F:15])[F:16])=[CH:11][CH:12]=3)[C:3]2=[O:17])[CH2:45][CH2:46]1)=[O:51])([CH3:56])([CH3:54])[CH3:55]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 11543684Tert-butyl 4-(2-hydroxyphenyl)piperazine-1-carboxylateHCID 21963156HCID 21963156、化合物HCID 51573101N-carboxylatoiminocarbamate

生成物 1

HCID 21963144HCID 21963144、化合物収率 64.4%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

To a 100 mL round-bottomed flask equipped with condenser and N2 inlet were added 241 mg (0.983 mmol) 3-hydroxy-1-(4-trifluoromethyl-phenyl)-pyrrolidin-2-one, 15 mL dry tetrahydrofuran, 645 mg (2.45 mmol) triphenylphosphine, and 328 mg (1.18 mmol) N-(2-hydroxyphenyl)-4-t-butoxycarbonyl-piperazine. A solution of 398 mg (1.97 mmol) disopropyl azodicarboxylate in 10 mL dry tetrahydrofuran was added dropwise over 5 minutes, and the reaction stirred at room temperature overnight. The reaction was quenched with aqueous sodium bicarbonate solution, separated, and the aqueous layer extracted three times with ethyl acetate. The combined organic layers were dried over magnesium sulfate and evaporated. The residue was chromatographed on silica using hexane/ethyl acetate as eluant to afford 320 mg (64%) of an oil.

後処理

  1. customTo a 100 mL round-bottomed flask equipped with condenser and N2 inlet
  2. customThe reaction was quenched with aqueous sodium bicarbonate solution
  3. customseparated
  4. extractionthe aqueous layer extracted three times with ethyl acetate
  5. dry with materialThe combined organic layers were dried over magnesium sulfate
  6. customevaporated
  7. customThe residue was chromatographed on silica

出典と根拠

ORDレコード
ord-a1f52a8665fa4ff2a436ff2e2f708639
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07101885B2

反応ノート

読み込み中…

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