Hydrochloric Acid → 2-(5-Bromothiophen-2-yl)ethan-1-amine--hydrogen chloride (1/1)

HRID 2412658ノート

反応式

HRID 2412658 の反応式
[Br:1][C:2]1[S:6][C:5]([CH2:7][CH2:8][NH:9]P(=O)(OCC)OCC)=[CH:4][CH:3]=1.C(OC(C)C)(C)C.[ClH:25].P(N)(=O)([O-])[O-]>>[ClH:25].[Br:1][C:2]1[S:6][C:5]([CH2:7][CH2:8][NH2:9])=[CH:4][CH:3]=1

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 7914Diisopropyl EtherHCID 211207Phosphoramidic acid, ion(2-)HCID 13740538diethyl N-[2-(5-bromothien-2-yl)-ethyl]-phosphoramidate

生成物 1

HCID 131315592-(5-Bromothiophen-2-yl)ethan-1-amine--hydrogen chloride (1/1)収率 60%

実験手順

A solution containing 3.42 g. (0.01 mol) diethyl N-[2-(5-bromothien-2-yl)-ethyl]-phosphoramidate in 50 ml. diisopropyl ether saturated with hydrogen chloride is stirred overnight at ambient temperature. The crystals formed are filtered off and washed with diisopropyl ether. After drying, there is obtained 1.45 g. (yield: 60%, referred to the phosphoramidate used) of the desired product in the form of silverygrey flakes; m.p. 220° C. (decomposition)

後処理

  1. additionA solution containing 3.42 g
  2. customThe crystals formed
  3. filtrationare filtered off
  4. washwashed with diisopropyl ether
  5. customAfter drying
  6. customthere is obtained 1.45 g

出典と根拠

ORDレコード
ord-27c98e0b85574fae9430a1f6c1868a03
出典データセット
uspto-grants-1985_01
特許番号
US04493931

反応ノート

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