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Benzylamine → 2-((Benzylamino)methyl)-2,3-dihydro-7H-[1,4]dioxino[2,3-e]indol-8(9H)-one

HRID 1737412
ノート
印刷プレビュー

反応式

HRID 1737412 の反応式
C1(C)C=CC(S(O[CH2:11][C@H:12]2[O:25][C:16]3=[C:17]4[C:21](=[CH:22][CH:23]=[C:15]3[O:14][CH2:13]2)[NH:20][C:19](=[O:24])[CH2:18]4)(=O)=O)=CC=1.S(C1C=CC(C)=CC=1)(OC[C@@H]1OC1)(=O)=O.[CH2:42]([NH2:49])[C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1>CS(C)=O>[CH2:42]([NH:49][CH2:11][CH:12]1[O:25][C:16]2=[C:17]3[C:21](=[CH:22][CH:23]=[C:15]2[O:14][CH2:13]1)[NH:20][C:19](=[O:24])[CH2:18]3)[C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7504BenzylamineHCID 154187Glycidyl tosylate, (R)-HCID 86754567(S)-2-(Toluene-4-sulfonyloxymethyl)-2,3,8,9-tetrahydro-7H-1,4-dioxino[2,3-e]indol-8-one

生成物 1

HCID 99103252-((Benzylamino)methyl)-2,3-dihydro-7H-[1,4]dioxino[2,3-e]indol-8(9H)-one

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
77.5 °C

実験手順

(S)-2-(Toluene-4-sulfonyloxymethyl)-2,3,8,9-tetrahydro-7H-1,4-dioxino[2,3-e]indol-8-one (2.0 g, 5.3 mmole), prepared in the same manner as the (R) enantiomer described above with substitution of (S)- for (R)-glycidyl tosylate, and benzylamine (2.9 ml, 26.7 mmole) were placed in 20 ml of fresh DMSO under nitrogen. The mixture was then heated to 75-80° C. with stirring for 3 hours. After cooling to room temperature, the reaction mixture was partitioned between ethyl acetate and brine. The DMSO layer was extracted with ethyl acetate and the combined ethyl acetate extracts were washed with water to remove trace DMSO, dried over anhydrous sodium sulfate and concentrated in vacuum. The residue was chromatographed on a silica gel column using ethyl acetate as the eluant to yield the free base (1.4 g, 4.5 mmole, 83%) of the expected product as a solidified oil under reduced pressure. The free base was dissolved in 20 ml of ethanol, treated with 0.25 M ethanolic fumaric acid (10 ml) and precipitated with diethyl ether to give the title compound as a pale yellow solid fumarate salt, predominantly in the (R)-configuration, m.p. 195-196° C. This sample, from which the pharmacological results reported in this application were obtained, was determined by chiral HPLC to contain 9% of the (S)-enantiomer.

後処理

  1. temperatureAfter cooling to room temperature
  2. customthe reaction mixture was partitioned between ethyl acetate and brine
  3. extractionThe DMSO layer was extracted with ethyl acetate
  4. washthe combined ethyl acetate extracts were washed with water
  5. customto remove trace DMSO
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuum
  8. customThe residue was chromatographed on a silica gel column

出典と根拠

ORDレコード
ord-7fb6a49e1639458cb49455d1c17a33b2
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05962465

反応ノート

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