Potassium sodium tartarate → HCID 22338185, 화합물

HRID 853042노트

반응식

HRID 853042 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C(O[C:10]([C:12]1[N:13]([CH2:22][C:23]#[N:24])[C:14]2[C:19]([CH:20]=1)=[C:18]([Br:21])[CH:17]=[CH:16][CH:15]=2)=O)C.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C(OCC)C>[Br:21][C:18]1[C:19]2[CH:20]=[C:12]3[CH2:10][NH:24][CH2:23][CH2:22][N:13]3[C:14]=2[CH:15]=[CH:16][CH:17]=1

참가 물질

5

반응물 3

HCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 694154234-bromo-1-cyanomethyl-1H-indole-2-carboxylic acid ethyl ester

생성물 1

HCID 22338185HCID 22338185, 화합물수율 34.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Lithium aluminiumhydride (4.0 g, 106 mmol) was suspended in diethylether (600 mL) and 4-bromo-1-cyanomethyl-1H-indole-2-carboxylic acid ethyl ester (13.0 g, 42 mmol) was added in portions. The mixture was boiled for 15 h, cooled to room temperature and added to saturated potassium sodium tartrate solution. Thorough washing of the filter-cake with ethyl acetate followed the filtration over Celite® to remove solids. The phases of the filtrate were separated and the water phase was extracted with ethylacetate. The organic phases were pooled, washed with brine, dried with MgSO4 and the solvent was evaporated. Chromatography on silica gel (dichloromethane/methanol 95:5) yielded 9-bromo-1,2,3,4-tetrahydro-pyrazino[1,2-a]indole (3.6 g, 34 %) as a colorless solid, MS: m/e=250.0 (M+).

후처리

  1. washThorough washing of the
  2. filtrationfilter-cake with ethyl acetate
  3. filtrationthe filtration over Celite®
  4. customto remove solids
  5. customThe phases of the filtrate were separated
  6. extractionthe water phase was extracted with ethylacetate
  7. washwashed with brine
  8. dry with materialdried with MgSO4
  9. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-3bf1bfad3f994b65aa21ebf4a48369cd
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253281B2

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