Hydrogen Sulfide → HCID 178519008, 화합물

HRID 610612노트

반응식

HRID 610612 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 178519008HCID 178519008, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5756fdafaf04494883e5753df9312e9c
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998613

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