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反応

Hydrochloric Acid → (S)-3-(4-piperazin-1-ylmethyl-phenyl)-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine

HRID 1841979

印刷プレビュー

反応式

HRID 1841979 の反応式

C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C@@H:21]3[O:30][C:25]4=[N:26][CH:27]=[CH:28][CH:29]=[C:24]4[O:23][CH2:22]3)=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.O.C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1>[N:11]1([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C@@H:21]3[O:30][C:25]4=[N:26][CH:27]=[CH:28][CH:29]=[C:24]4[O:23][CH2:22]3)=[CH:17][CH:16]=2)[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

参加物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 313Hydrochloric Acid

HCID 10340Sodium Carbonate

HCID 866953624-[(S)-4-(2,3-Dihydro-[1,4]dioxino[2,3-b]pyridin-3-yl)-benzyl]-piperazine-1-carboxylic acid tert-butyl ester2 回

生成物 1

HCID 86695358(S)-3-(4-piperazin-1-ylmethyl-phenyl)-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine

試薬・触媒・溶媒 1

HCID 31275

1,4-Dioxane

溶媒

2 回

実験手順

To a solution of 4-[(S)-4-(2,3-dihydro-[1,4]dioxino[2,3-b]pyridin-3-yl)-benzyl]-piperazine-1-carboxylic acid tert-butyl ester (prepared from Intermediate C and piperazine-1-carboxylic acid tert-butyl ester according to General Method N) (7.32 g, 17.8 mmol) in 1,4-dioxane (200 mL) is added 4M HCl in 1,4-dioxane (22.2 mL, 88.9 mmol). The resulting slurry is stirred overnight. The reaction is poured into water (600 mL) and basified with 2M aqueous Na2CO3. The product is extracted with DCM, and the combined extracts washed with brine and dried over Na2SO4 to afford the title compound (S) as an oil that partially crystallizes.

後処理

extractionThe product is extracted with DCM
washthe combined extracts washed with brine
dry with materialdried over Na2SO4

出典と根拠

ORDレコード: ord-4a4943d2ae7f474abe816fdcd40812af
出典データセット: uspto-grants-2015_02
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08946203B2

反応ノート

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