Hydrogen Sulfide → HCID 178519008、化合物

HRID 566457ノート

反応式

HRID 566457 の反応式
C(N[C:9]1[CH2:17][CH2:16][CH2:15][CH2:14][C:10]=1[C:11]([NH2:13])=[O:12])C1C=CC=CC=1.[SH2:18]>C(O)(=O)C>[OH:12][C:11]1[C:10]2[CH2:14][CH2:15][CH2:16][CH2:17][C:9]=2[S:18][N:13]=1

参加物

4

反応物 2

HCID 402Hydrogen SulfideHCID 106571002-(Benzylamino)-3,4,5,6-tetrahydrobenzamide

生成物 1

HCID 178519008HCID 178519008、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 2-benzylamino-3,4,5,6-tetrahydrobenzamide 21a (15 g) in glacial acetic acid (100 mL) was added excess hydrogen sulfide at 80° C. for 4 h. The reaction mixture was evaporated and ether was added to the residue which afforded crystallisation. The crystals were dissolved in ethyl acetate (30 mL) and a solution of bromine (8.3 mL) in ethyl acetate (30 mL) was dropwise added at room temperature. The mixture was stirred for 20 h at room temperature and evaporated. Column chromatography on silica gel (eluent: ethyl acetate-ethanol 1:1 containing 1% glacial acetic acid) gave the title compound (3.3 g): mp 157-158° C.

後処理

  1. customThe reaction mixture was evaporated
  2. additionether was added to the residue which
  3. customafforded
  4. customcrystallisation
  5. dissolutionThe crystals were dissolved in ethyl acetate (30 mL)
  6. additiona solution of bromine (8.3 mL) in ethyl acetate (30 mL) was dropwise added at room temperature
  7. customevaporated

出典と根拠

ORDレコード
ord-9b9c024b17884870aeef7f26aeda20ce
出典データセット
uspto-grants-2001_01
特許番号
US06174909B1

反応ノート

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