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Triphenylphosphine → Methyl 2-(1-tert-Butoxycarbonylpiperidin-4-yloxy)-4-fluorobenzoate

HRID 1787889
ノート
印刷プレビュー

反応式

HRID 1787889 の反応式
[F:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([OH:12])[CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:32]([O:36][C:37]([N:39]1[CH2:44][CH2:43][CH:42](O)[CH2:41][CH2:40]1)=[O:38])([CH3:35])([CH3:34])[CH3:33].N(C(OCC)=O)=NC(OCC)=O>C(Cl)Cl.C1C=CC=CC=1>[C:32]([O:36][C:37]([N:39]1[CH2:44][CH2:43][CH:42]([O:12][C:4]2[CH:3]=[C:2]([F:1])[CH:11]=[CH:10][C:5]=2[C:6]([O:8][CH3:9])=[O:7])[CH2:41][CH2:40]1)=[O:38])([CH3:35])([CH3:33])[CH3:34]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 643502Tert-butyl 4-hydroxypiperidine-1-carboxylateHCID 2775386Methyl 4-fluorosalicylate

生成物 1

HCID 57602502Methyl 2-(1-tert-Butoxycarbonylpiperidin-4-yloxy)-4-fluorobenzoate収率 61%

試薬・触媒・溶媒 2

HCID 241
Benzene
溶媒
HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A mixture of methyl 4-fluoro-2-hydroxybenzoate (5.1 g, 30 mmol), triphenylphosphine (9.5 g, 36 mmol), 1-tert-butoxycarbonyl-4-hydroxypiperidine (6 g, 30 mmol), and benzene (10 mL) was heated until all solids dissolved. The solution was cooled to 0° C., then sonicated while adding diethyl azodicarboxylate (6.3 g, 36 mmol) dropwise. After the addition was complete, the reaction mixture was sonicated for an additional 60 min, diluted with CH2Cl2 (25 mL), and purified by flash chromatography, eluting with 10% EtOAc in hexanes to yield the title compound (6.45 g, 61%) as a white solid.

後処理

  1. temperaturewas heated until all solids
  2. dissolutiondissolved
  3. customsonicated
  4. additionAfter the addition
  5. customthe reaction mixture was sonicated for an additional 60 min
  6. custompurified by flash chromatography
  7. washeluting with 10% EtOAc in hexanes

出典と根拠

ORDレコード
ord-5b54b93e44bc459fb114f8396288f7b7
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07511066B2

反応ノート

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