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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0

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反応

2,2'-Bipyridine → 2-Trifluoromethyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester

HRID 2237449

印刷プレビュー

反応式

HRID 2237449 の反応式

C(O[C:4](=O)[CH2:5][N:6]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:7][CH2:8][C:9]1[S:10][CH:11]=[CH:12][CH:13]=1)C.N1C=CC=CC=1C1C=CC=CN=1.[F-].[K+].C[Si]([C:38]([F:41])([F:40])[F:39])(C)C>CN(C=O)C.[Cu]I.CN1C(=O)CCC1>[CH2:17]([O:16][C:14]([N:6]1[CH2:5][CH2:4][C:13]2[CH:12]=[C:11]([C:38]([F:41])([F:40])[F:39])[S:10][C:9]=2[CH2:8][CH2:7]1)=[O:15])[CH3:18]

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 14742,2'-Bipyridine

HCID 522689Potassium Fluoride

HCID 552549(Trifluoromethyl)trimethylsilane

HCID 66934051[Ethoxycarbonyl-(2-thiophen-2-yl-ethyl)-amino]acetic acid ethyl ester

生成物 1

HCID 684758472-Trifluoromethyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester

試薬・触媒・溶媒 3

HCID 24350

Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)

触媒

HCID 6228Dimethylformamide溶媒

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度: 80 °C

実験手順

A solution of the product from step a.) (75 mg, 0.21 mmol) in DMF (0.5 ml) and NMP (0.5 ml) was treated with bipyridyl (43 mg, 0.27 mmol), CuI (44 mg, 0.23 mmol), KF (13 mg, 0.23 mmol) and trimethylsilyltrifluoromethane (2.1 ml, 1.05 mmol). The reaction mixture was heated to 80° C. for 3 days. The reaction was cooled and filtered through celite washing with EtOAc (20 ml). The eluent was washed with brine (2×3 ml) and dried (MgSO4) providing the subtitle compound as a brown oil that was used without further purification.

後処理

temperatureThe reaction was cooled
filtrationfiltered
washthrough celite washing with EtOAc (20 ml)
washThe eluent was washed with brine (2×3 ml)
dry with materialdried (MgSO4)

出典と根拠

ORDレコード: ord-2bdb7c26d0cb4058bb29788725dfe7de
出典データセット: uspto-grants-2010_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07718647B2

反応ノート

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