Triethylamine → HCID 44544857、化合物

HRID 391255ノート

反応式

HRID 391255 の反応式
S(Cl)(Cl)=O.[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]([OH:15])=[O:14].S(Cl)([Cl:19])(=O)=O.[O:21]=[C:22]([N:26]1[CH2:30][CH2:29][CH2:28][CH2:27]1)[C@H:23](O)[CH3:24].C(N(CC)CC)C>O.C1(C)C=CC=CC=1>[Cl:19][CH:12]([C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[Cl:5])[C:13]([O:15][C@H:23]([CH3:24])[C:22](=[O:21])[N:26]1[CH2:30][CH2:29][CH2:28][CH2:27]1)=[O:14]

参加物

8

反応物 5

HCID 8471TriethylamineHCID 17124o-Chlorophenylacetic acidHCID 24386Thionyl ChlorideHCID 24648Sulfuryl chlorideHCID 11194401Pyrrolidine, 1-[(2R)-2-hydroxy-1-oxopropyl]- (9CI)

生成物 1

HCID 44544857HCID 44544857、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 1140Toluene溶媒

反応条件

温度
50 °C

実験手順

To thionyl chloride (7.7 g, 64.7 mmol), 2-chlorophenylacetic acid (10 g, 58.6 mmol) was added. The mixture was stirred at 50° C. for 3 hours. After stirring, sulfuryl chloride (12.7 g, 93.8 mmol) was added thereto at the same temperature for reaction overnight. After the reaction, toluene (45 mL) was added and (2R)-1-oxo-1-pyrrolidinylpropane-2-ol (9.2 g, 64.5 mmol) was added thereto at the same temperature. Subsequently, triethylamine (7.7 g, 93.8 mmol) was added to carry out reaction for 2 hours. After the reaction, water was added thereto and the water layer was disposed of. The obtained organic layer was washed with water, and the water layer was disposed of. The organic layer was concentrated under reduced pressure to obtain 19 g of the concentrate of the target compound.

後処理

  1. stirringAfter stirring
  2. customat the same temperature for reaction overnight
  3. additionwas added
  4. customreaction for 2 hours
  5. additionwas added
  6. washThe obtained organic layer was washed with water
  7. concentrationThe organic layer was concentrated under reduced pressure
  8. customto obtain 19 g of the
  9. concentrationconcentrate of the target compound

出典と根拠

ORDレコード
ord-7302bdd5c36e44e8b1d26a44d29f3500
出典データセット
uspto-grants-2013_02
特許番号
US08383833B2

反応ノート

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