Hydrochloric Acid → Ethyl 2-(aminomethyl)-5-fluorobenzoate hydrochloride

HRID 455291ノート

反応式

HRID 455291 の反応式
[ClH:1].C(OC([NH:9][CH2:10][C:11]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:12]=1[C:13]([O-:15])=[O:14])=O)(C)(C)C.[CH2:21]1COC[CH2:22]1>>[ClH:1].[NH2:9][CH2:10][C:11]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:12]=1[C:13]([O:15][CH2:21][CH3:22])=[O:14]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 866675072-((Tert-butoxycarbonylamino)methyl)-5-fluorobenzoate

生成物 1

HCID 67109674Ethyl 2-(aminomethyl)-5-fluorobenzoate hydrochloride

反応条件

温度
50 °C

実験手順

Concentrated HCl (37%; 16 ml) was added dropwise to a solution of thyl 2-((tert-butoxycarbonylamino)methyl)-5-fluorobenzoate (Example 3; 15.9 g; 53.6 mmol) in THF (96 ml). The mixture was heated at 50° C. for 2 hours. The mixture was concentrated to dryness. The residue was taken up in ethanol (200 ml) and concentrated again. The solid was triturated from ether (100 ml). The precipitate was filtered off and washed with diethyl ether (2×50 ml).

後処理

  1. concentrationThe mixture was concentrated to dryness
  2. concentrationconcentrated again
  3. customThe solid was triturated from ether (100 ml)
  4. filtrationThe precipitate was filtered off
  5. washwashed with diethyl ether (2×50 ml)

出典と根拠

ORDレコード
ord-ebd0173aa2fb4a64ab8da0b4ff32eadb
出典データセット
uspto-grants-2013_07
特許番号
US08497270B2

反応ノート

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