Thionyl Chloride → HCID 54025343, 화합물

HRID 1288166노트

반응식

HRID 1288166 반응식
[CH2:1]([O:3][C:4]([N:6]1[CH2:20][CH2:19][C:18]2[C:9](=[N:10][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=3[C:17]=2[CH3:21])[CH:8](O)[CH2:7]1)=[O:5])[CH3:2].S(Cl)([Cl:25])=O>>[CH2:1]([O:3][C:4]([N:6]1[CH2:20][CH2:19][C:18]2[C:9](=[N:10][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=3[C:17]=2[CH3:21])[CH:8]([Cl:25])[CH2:7]1)=[O:5])[CH3:2]

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 53875304HCID 53875304, 화합물

생성물 1

HCID 54025343HCID 54025343, 화합물

실험 절차

1 gm (3.3 millimols) of 5-hydroxy-1,2,4,5-tetrahydro-11methyl-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester was stirred for 2 hours with 20 ml of thionyl chloride at room temperature. The excess thionyl chloride was then distilled off in vacuo, the residue was dissolved in chloroform, the solution was dried with sodium sulfate, and the solvent was distilled off. After purification of the residue on a silicagel column with benzene/ethyl acetate (8:2) as the eluant, the yield was 0.55 gm (52% of theory), m.p. 131° C.

후처리

  1. distillationThe excess thionyl chloride was then distilled off in vacuo
  2. dissolutionthe residue was dissolved in chloroform
  3. dry with materialthe solution was dried with sodium sulfate
  4. distillationthe solvent was distilled off
  5. customAfter purification of the residue on a silicagel column with benzene/ethyl acetate (8:2) as the eluant

출처 및 근거

ORD 기록
ord-9adbbbdbf2a241d3aad2826b7091c370
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03987047

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