Methyl iodide → HCID 86741154, 화합물

HRID 1249084노트

반응식

HRID 1249084 반응식
[CH2:1]([C@H:4]1[C:16]2[NH:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[C:8]=2[CH2:7][C@@H:6]([C:17]([OH:19])=[O:18])[NH:5]1)[CH2:2][CH3:3].C(N(CC)CC)C.[C:27](=[S:29])=[S:28].[CH3:30]I>CO>[CH2:1]([C@H:4]1[C:16]2[NH:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[C:8]=2[CH2:7][C@@H:6]([C:17]([OH:19])=[O:18])[N:5]1[C:27]([S:29][CH3:30])=[S:28])[CH2:2][CH3:3]

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 762190HCID 762190, 화합물

생성물 1

HCID 86741154HCID 86741154, 화합물수율 59%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(1RS,3RS)-cis-n-Propyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid (450 mg) is dissolved in 80% methanol (10 ml), and thereto are added triethylamine (350 mg) and carbon disulfide (270 ml). The mixture is stirred at room temperature for 30 minutes, and methyl iodide (490 mg) is added to the mixture. The mixture is stirred at room temperature for 2 hours, and then distilled to remove the solvent. Water is added to the mixture, and the aqueous solution is acidified with 5% HCl, and extracted with ethyl acetate. The extract is washed with water, dried and then distilled to remove the solvent. The residue is treated with aqueous ethanol to give the title compound (350 mg, 59%) as pale yellow powder.

후처리

  1. stirringThe mixture is stirred at room temperature for 2 hours
  2. distillationdistilled
  3. customto remove the solvent
  4. additionWater is added to the mixture
  5. extractionextracted with ethyl acetate
  6. washThe extract is washed with water
  7. customdried
  8. distillationdistilled
  9. customto remove the solvent
  10. additionThe residue is treated with aqueous ethanol

출처 및 근거

ORD 기록
ord-a4f143ac1d704fee9edee32dad97840d
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04628057

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