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Benzophenone imine → tert-Butyl 3-(6-(Diphenylmethyleneamino)pyridin-3-yl)azetidine-1-carboxylate

HRID 1772128
ノート
印刷プレビュー

反応式

HRID 1772128 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([CH:8]2[CH2:11][N:10]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:9]2)=[CH:4][CH:3]=1.[C:19](=[NH:32])([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.CC(C)([O-])C.[Na+].C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Pd].[Pd].C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1>[C:20]1([C:19](=[N:32][C:2]2[N:7]=[CH:6][C:5]([CH:8]3[CH2:11][N:10]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:9]3)=[CH:4][CH:3]=2)[C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
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

6

反応物 4

HCID 136809Benzophenone imineHCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 57537370Tert-butyl 3-(6-chloropyridin-3-yl)azetidine-1-carboxylate

生成物 1

HCID 86697066tert-Butyl 3-(6-(Diphenylmethyleneamino)pyridin-3-yl)azetidine-1-carboxylate収率 79.1%

試薬・触媒・溶媒 1

HCID 76545419
Dibenzylideneacetone dipalladium
触媒

反応条件

温度
100 °C

実験手順

A 500-mL round-bottomed flask equipped with a magnetic stirrer and reflux condenser was charged with 117a (2.00 g, 7.46 mmol), benzophenoneimine (1.62 g, 8.96 mmol), sodium tert-butoxide (1.00 g, 10.4 mmol), (dibenzylideneacetone)-dipalladium(0) (340 mg, 0.373 mmol) and rac-2,2′-bis(diphenylphosphino)-1,1′-binapthyl (700 mg, 1.12 mmol), and the reaction was heated at 100° C. for 3 h. After this time the reaction was cooled to room temperature and concentrated under reduced pressure. The resulting oil was purified by column chromatography to afford a 79% yield (2.44 g) of 117b as a brown solid: mp 104-105° C.; 1H NMR (500 MHz, CDCl3) δ 8.20 (d, 1H, J=2.0 Hz), 7.85 (br s, 2H), 7.52 (br s, 1H), 7.44 (br s, 2H), 7.47 (dd, 1H, J=8.5, 2.0 Hz), 7.17 (br s, 5H), 6.61 (d, 1H, J=8.5 Hz), 4.30 (t, 2H, J=8.5 Hz), 3.86 (dd, 2H, J=8.5, 4.5 Hz), 3.62 (m, 1H), 1.45 (s, 9H); MS (ESI+) m/z 413.8 (M+H).

後処理

  1. customA 500-mL round-bottomed flask equipped with a magnetic stirrer
  2. temperaturereflux condenser
  3. temperatureAfter this time the reaction was cooled to room temperature
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting oil was purified by column chromatography

出典と根拠

ORDレコード
ord-2b2bccff976849edb0ea5e3553233529
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09249123B2

反応ノート

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