Water → 6-Acety-3-(2-bromoethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine

HRID 1734042

반응식

HRID 1734042 반응식
[C:1]([N:4]1[CH2:9][CH2:8][C:7]2[C:10]([C:14](=O)[CH2:15][Br:16])=[C:11]([CH3:13])[S:12][C:6]=2[CH2:5]1)(=[O:3])[CH3:2].O>C([SiH](CC)CC)C.FC(F)(F)C(O)=O>[C:1]([N:4]1[CH2:9][CH2:8][C:7]2[C:10]([CH2:14][CH2:15][Br:16])=[C:11]([CH3:13])[S:12][C:6]=2[CH2:5]1)(=[O:3])[CH3:2]

참가 물질

5

반응물 2

HCID 962WaterHCID 21471958HCID 21471958, 화합물

생성물 1

HCID 214719356-Acety-3-(2-bromoethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine수율 52.3%

시약·촉매·용매 2

HCID 6422Trifluoroacetic acid용매HCID 12052Triethylsilane용매

실험 절차

A mixture of 28 g of 6-acetyl-3-bromoacetyl-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine in 42 ml of triethylsilane and 140 ml of trifluoroacetic acid was stirred at room temperature for 5 hours. The mixture was poured into water, made alkaline and extracted with ethyl acetate. The organic layer was washed with water, dried and concentrated. To the residue was added isopropyl ether and the precipitated crystals were collected by filtration to give 14 g of 6-acetyl-3-(2-bromoethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine as white crystals, m.p. 93°-95° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationconcentrated
  5. additionTo the residue was added isopropyl ether
  6. filtrationthe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-54977645a3514bc2aa29664f22a1d46a
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532240

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