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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

Dichloromethane → 3-(Tert-butyldimethylsilyloxy)-1-(3,4-difluorophenyl)propan-1-amine

HRID 2279542

印刷プレビュー

反応式

HRID 2279542 の反応式

[NH2:1][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([F:12])=[C:8]([F:13])[CH:7]=1)[CH2:3][CH2:4][OH:5].[CH3:14][C:15]([Si:18](Cl)([CH3:20])[CH3:19])([CH3:17])[CH3:16].CCN(C(C)C)C(C)C.C(Cl)Cl>CN(C1C=CN=CC=1)C.O>[Si:18]([O:5][CH2:4][CH2:3][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([F:12])=[C:8]([F:13])[CH:7]=1)[NH2:1])([C:15]([CH3:17])([CH3:16])[CH3:14])([CH3:20])[CH3:19]

参加物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 6344Dichloromethane

HCID 28928tert-Butyldimethylsilyl chloride

HCID 81531Diisopropylethylamine

HCID 623897353-Amino-3-(3,4-difluorophenyl)propan-1-ol

生成物 1

HCID 682943123-(Tert-butyldimethylsilyloxy)-1-(3,4-difluorophenyl)propan-1-amine収率 69.9%

試薬・触媒・溶媒 2

HCID 14284

4-(Dimethylamino)pyridine

触媒

HCID 962Water溶媒

実験手順

A solution of 304 (0.400 g, 2.14 mmol), TBDMS-Cl (0.386 g, 2.56 mmol), DIPEA (0.744 mL, 4.27 mmol), DMAP (0.0261 g, 0.214 mmol) and DCM (10 mL) was stirred at RT for 1 h and then poured into water and extracted with DCM. The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with DCM/MeOH (500:7) to afford 0.45 g (69.9%) of 3-(tert-butyldimethylsilyloxy)-1-(3,4-difluorophenyl)propan-1-amine (306).

後処理

extractionextracted with DCM
dry with materialThe combined organic extracts were dried (MgSO4)
filtrationfiltered
concentrationconcentrated in vacuo
customThe crude product was purified by SiO2 chromatography
washeluting with DCM/MeOH (500:7)

出典と根拠

ORDレコード: ord-f64a70a54dfb425a98a88cc59d9d4b4e
出典データセット: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09133187B2

反応ノート

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