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Thionyl Chloride → 3-Benzo[1,3]dioxol-5-ylpiperidin-1-yl-(R)-2,3-dihydrobenzo[1,4]dioxin-2-ylmethanone

HRID 2365968
ノート
印刷プレビュー

反応式

HRID 2365968 の反応式
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][C@@H:2]1[C:11]([OH:13])=O.S(Cl)(Cl)=O.Cl.[O:19]1[C:23]2[CH:24]=[CH:25][C:26]([CH:28]3[CH2:33][CH2:32][CH2:31][NH:30][CH2:29]3)=[CH:27][C:22]=2[O:21][CH2:20]1.CCN(C(C)C)C(C)C>C(Cl)Cl.O.C1(C)C=CC=CC=1>[O:19]1[C:23]2[CH:24]=[CH:25][C:26]([CH:28]3[CH2:33][CH2:32][CH2:31][N:30]([C:11]([C@@H:2]4[O:1][C:6]5[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=5[O:4][CH2:3]4)=[O:13])[CH2:29]3)=[CH:27][C:22]=2[O:21][CH2:20]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

8

反応物 4

HCID 24386Thionyl ChlorideHCID 81531DiisopropylethylamineHCID 687062(R)-1,4-Benzodioxane-2-carboxylic acidHCID 667274853-benzo[1,3]dioxol-5-yl-piperidine HCl

生成物 1

HCID 667272583-Benzo[1,3]dioxol-5-ylpiperidin-1-yl-(R)-2,3-dihydrobenzo[1,4]dioxin-2-ylmethanone収率 84.9%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 1140Toluene溶媒
HCID 6344Dichloromethane溶媒

反応条件

温度
95 °C

実験手順

A mixture of (R)-2,3-dihydrobenzo[1,4]dioxine-2-carboxylic acid (167 mg, 0.93 mmol), thionyl chloride (338 μl, 551 mg, 4.63 mmol) and dry toluene was heated at 95° C. for 1.5 h and then evaporated to dryness. Toluene was added and the evaporation was repeated. The evaporation residue was dissolved in DCM (2 ml) and added slowly to a cold solution (0° C.) of 3-benzo[1,3]dioxol-5-yl-piperidine HCl (224 mg, 0.93 mmol) and DIPEA (0.324 ml, 240 mg, 1.85 mmol) in DCM (5 ml). The reaction mixture was stirred for 1 h 45 min at RT. Water was added, layers were separated and the organic phase was washed twice with 1 M HCl and sat. NaHCO3. The organic phase was dried (Na2SO4), filtered and evaporated to give 290 mg of the title compound.

後処理

  1. customevaporated to dryness
  2. additionToluene was added
  3. customthe evaporation
  4. dissolutionThe evaporation residue was dissolved in DCM (2 ml)
  5. customlayers were separated
  6. washthe organic phase was washed twice with 1 M HCl and sat. NaHCO3
  7. dry with materialThe organic phase was dried (Na2SO4)
  8. filtrationfiltered
  9. customevaporated

出典と根拠

ORDレコード
ord-cee0d6bfafa740eeb322a8cc30f415ed
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697723B2

反応ノート

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