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Hydrochloric Acid → M-58996

HRID 967787
ノート
印刷プレビュー

反応式

HRID 967787 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][C:14]([CH2:18][N:19]([CH3:33])[C:20]3[CH:32]=[CH:31][C:23]([C:24]([O:26]C(C)(C)C)=[O:25])=[CH:22][CH:21]=3)([OH:17])[CH2:13][CH2:12]2)=[CH:5][CH:4]=1)#[N:2].O.C(=O)([O-])[O-].[K+].[K+].[ClH:41]>>[ClH:41].[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][C:14]([CH2:18][N:19]([CH3:33])[C:20]3[CH:21]=[CH:22][C:23]([C:24]([OH:26])=[O:25])=[CH:31][CH:32]=3)([OH:17])[CH2:15][CH2:16]2)=[CH:7][CH:8]=1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 11430Potassium CarbonateHCID 22930217Tert-butyl 4-({1-[2-(4-cyanophenyl)ethyl]-4-hydroxypiperidin-4-ylmethyl}methylamino)benzoate

生成物 1

HCID 67371796M-58996

実験手順

The compound (100 mg) obtained in Step 2 of Example 21 was dissolved in 6N hydrochloric acid (0.5 mL) at room temperature and stirred at the same temperature for five hours. To the mixture was added water (3 mL) and adjusted to pH 9 to 10 by potassium carbonate, and the aqueous layer was washed with ethyl acetate. Insoluble matter of the aqueous layer was removed by filtration and the filtrate was adjusted to pH 3 with 6N hydrochloric acid. The precipitate was collected by filtration and dried to obtain the titled compound (71 mg) as crystals. The physical data of the obtained compound accord with those of the compound of Example 29.

後処理

  1. washthe aqueous layer was washed with ethyl acetate
  2. customInsoluble matter of the aqueous layer was removed by filtration
  3. filtrationThe precipitate was collected by filtration
  4. customdried

出典と根拠

ORDレコード
ord-73f1b51b37c54a48a8b1e71ce9bc6bd0
出典データセット
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06956046B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート