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Water → tert-butyl 8-(cyclohexyloxy)-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate

HRID 2191260
ノート
印刷プレビュー

反応式

HRID 2191260 の反応式
[CH:1]1([OH:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].Cl[C:11]1[CH:12]=[CH:13][C:14]2[CH2:15][N:16]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:17][CH2:18][O:19][C:20]=2[N:21]=1.O>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1>[CH:1]1([O:7][C:11]2[CH:12]=[CH:13][C:14]3[CH2:15][N:16]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:17][CH2:18][O:19][C:20]=3[N:21]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]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

8

反応物 4

HCID 962WaterHCID 7966CyclohexanolHCID 24758Sodium hydrideHCID 57356939Tert-butyl 8-chloro-2,3-dihydropyrido[3,2-F][1,4]oxazepine-4(5H)-carboxylate

生成物 1

HCID 68430226tert-butyl 8-(cyclohexyloxy)-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate収率 65%

試薬・触媒・溶媒 3

HCID 634876
Binap, (A+-)-
触媒
HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 1140Toluene溶媒2 回

反応条件

温度
70 °C

実験手順

To a solution of cyclohexanol (0.19 mL) in toluene (4 mL) was added sodium hydride (0.14 g), and the resulting mixture was stirred at 70° C. for 15 min under a nitrogen atmosphere. A mixture of tert-butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (0.50 g), BINAP (0.033 g), Pd2(dba)3 (0.024 g) and toluene (4 mL) was added, and the resulting mixture was stirred at 100° C. for 2 hr under an argon atmosphere. The reaction solution was poured into water, and the resulting product was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (solvent gradient; 0→40% ethyl acetate/hexane) to give tert-butyl 8-(cyclohexyloxy)-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (0.40 g, 65%) as a colorless oil.

後処理

  1. additionwas added
  2. stirringthe resulting mixture was stirred at 100° C. for 2 hr under an argon atmosphere
  3. extractionthe resulting product was extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine
  5. customdried
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (solvent gradient; 0→40% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-b3a61cf58bee46c880b80578f20570c6
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329687B2

反応ノート

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