Hydrochloric Acid → 2-{2-[4-(4-Aminobutyl)phenoxy]ethylamino}acetamide dihydrochloride salt

HRID 1509863ノート

反応式

HRID 1509863 の反応式
C(OC(=O)[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][NH:21][CH2:22][C:23](=[O:25])[NH2:24])=[CH:14][CH:13]=1)(C)(C)C.[ClH:27]>C1COCC1.O1CCOCC1>[ClH:27].[ClH:27].[NH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][NH:21][CH2:22][C:23]([NH2:24])=[O:25])=[CH:14][CH:13]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 58809802(4-{4-[2-(Carbamoylmethylamino)ethoxy]phenyl}butyl)carbamic acid tert-butyl ester

生成物 1

HCID 668399752-{2-[4-(4-Aminobutyl)phenoxy]ethylamino}acetamide dihydrochloride salt

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 312751,4-Dioxane溶媒

実験手順

Compound 3 (0.25 g, 0.68 mmol) was dissolved in THF (3 mL), treated with 4 N HCl in dioxane (10 mL) and the reaction was stirred at room temperature for 2 hours. After this time, TLC analysis indicated a complete reaction. The reaction mixture was concentrated under vacuum, and methanol (2 mL) was added to the resulting residue. The resulting precipitate was collected by vacuum filtration and further dried in a vacuum oven to provide 4 (0.154 g, 67% overall yield for two steps) as a light brown solid. 1H NMR (300 MHz, CD3OD) δ 1.70 (m, 4H), 2.65 (m, 2H), 2.95 (m, 2H), 3.27 (m, 2H), 3.52 (t, 2H), 3.90 (s, 2H), 4.30 (t, 2H), 6.92 (d, 2H), 7.18 (d, 2H). m/z (ESI) 266.

後処理

  1. customa complete reaction
  2. concentrationThe reaction mixture was concentrated under vacuum, and methanol (2 mL)
  3. additionwas added to the resulting residue
  4. filtrationThe resulting precipitate was collected by vacuum filtration
  5. customfurther dried in a vacuum oven
  6. customto provide
  7. custom4 (0.154 g, 67% overall yield for two steps) as a light brown solid

出典と根拠

ORDレコード
ord-63f4a85769d14cfda1a9b7a5cbade9fc
出典データセット
uspto-grants-2012_07
特許番号
US08211895B2

反応ノート

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