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Triethylamine → HCID 16036824、化合物

HRID 2425510
ノート
印刷プレビュー

反応式

HRID 2425510 の反応式
[CH3:1][S:2][C:3]1[C:4]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[N:5][C:6]2[C:11]([C:12]=1[C:13]([OH:15])=O)=[CH:10][CH:9]=[CH:8][CH:7]=2.C(N(CC)CC)C.S(Cl)(Cl)=O.[C:33]1([C@@H:39]([NH2:42])[CH2:40][CH3:41])[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1>CCOC(C)=O.O>[CH3:1][S:2][C:3]1[C:4]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[N:5][C:6]2[C:11]([C:12]=1[C:13]([NH:42][C@H:39]([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)[CH2:40][CH3:41])=[O:15])=[CH:10][CH:9]=[CH:8][CH:7]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 291267HCID 291267、化合物HCID 6993773(1S)-1-phenylpropan-1-amine

生成物 1

HCID 16036824HCID 16036824、化合物収率 71.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8857
Ethyl Acetate
溶媒
2 回

実験手順

To a solution of 3-(methylthio)-2-phenylquinoline-4-carboxylic acid (150 mg, 0.51 mmol) and triethylamine (0.17 mL, 1.22 mmol) in EtOAc (2.5 mL) at 5° C. was added thionyl chloride (0.043 mL, 0.61 mmol). The cooling bath was removed and the suspension allowed to stir for 0.5 h, then (S)-(−)-1-phenylpropylamine (76 mg, 0.56 mmol) was added and reaction allowed to stir for another 0.5 h. Water (2 mL) and EtOAc (2 mL) were then added, the layers shaken together, then separated, the organics dried over Na2SO4, filtered, and concentrated under reduced pressure. The resulting material was purified by silica gel chromatography (0-20% EtOAc/CH2Cl2) to give the desired product (150 mg, 70% yield) as a solid. 1H NMR (300 MHz, CDCl3) δ 8.11 (d, J=8.4 Hz, 1H), 7.78-7.67 (m, 4H), 7.55-7.27 (m, 9H), 6.12 (d, J=8.5 Hz, 1H), 5.30 (q, J=7.6 Hz, 1H), 2.16-1.91 (m, 5H), 1.06 (t, J=7.4 Hz, 3H); HRMS m/z 413.1669, calcd 413.1688.

後処理

  1. customThe cooling bath was removed
  2. customreaction
  3. stirringto stir for another 0.5 h
  4. stirringthe layers shaken together
  5. customseparated
  6. dry with materialthe organics dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe resulting material was purified by silica gel chromatography (0-20% EtOAc/CH2Cl2)

出典と根拠

ORDレコード
ord-93ed41bef03d491084f0783ce34c2f63
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07964733B2

反応ノート

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