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Phosphorus oxychloride → HCID 178506080、化合物

HRID 1497235
ノート
印刷プレビュー

反応式

HRID 1497235 の反応式
[C:1]1([C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:17]([F:20])([F:19])[F:18])[CH:15]=3)[NH:10][C:9](=O)[C:8]=2[C:22]2[NH:26][N:25]=[N:24][N:23]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:29])=O.C(N(CC)C(C)C)(C)C>C1(C)C=CC=CC=1>[Cl:29][C:9]1[C:8]([C:22]2[NH:26][N:25]=[N:24][N:23]=2)=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:17]([F:19])([F:18])[F:20])[CH:15]=2)[N:10]=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 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 178518603HCID 178518603、化合物

生成物 1

HCID 178506080HCID 178506080、化合物収率 64%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
70 °C

実験手順

4-Phenyl-3-(1H-tetrazol-5-yl)-6-trifluoromethyl-1H-quinolin-2-one (160 mg, 448 μmol) was twice co-evaporated with toluene (5 ml). Then toluene (5 ml), phosphorus oxychloride (446 mg, 271 μl, 2.91 mmol) and N,N-diisopropylethylamine (72.3 mg, 97.8 μl, 560 μmol) were added and the mixture was heated to 70° C. for 5 h. Then all volatiles were removed and toluene (5 ml) was added and evaporated twice. Then ethanol (5 ml) was added and evaporated. Water and methanol were added to the remaining residue and the solid was filtered off and dried to obtain the title compound (107 mg, 64%) as brown solid. MS (ESI): 374.3 (M−H)−.

後処理

  1. customThen all volatiles were removed
  2. additiontoluene (5 ml) was added
  3. customevaporated twice
  4. additionThen ethanol (5 ml) was added
  5. customevaporated
  6. additionWater and methanol were added to the remaining residue
  7. filtrationthe solid was filtered off
  8. customdried

出典と根拠

ORDレコード
ord-eaf76f982fce4ad9bb5e6118a168ea36
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09199938B2

反応ノート

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