Methanesulfonyl isocyanate → HCID 13768039、化合物

HRID 1789354ノート

反応式

HRID 1789354 の反応式
[F:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][O:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[CH:23]3[NH:27][CH2:26][CH2:25][S:24]3)[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.[CH3:28][S:29]([N:32]=[C:33]=[O:34])(=[O:31])=[O:30]>CC(C)=O>[CH3:28][S:29]([NH:32][C:33]([N:27]1[CH2:26][CH2:25][S:24][CH:23]1[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[O:16][CH2:15][CH2:14][N:11]1[CH2:12][CH2:13][N:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=2)[CH2:9][CH2:10]1)=[O:34])(=[O:31])=[O:30]

参加物

4

反応物 2

HCID 12668338Methanesulfonyl isocyanateHCID 13768101HCID 13768101、化合物

生成物 1

HCID 13768039HCID 13768039、化合物収率 61.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

1.94 g of 2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine are dissolved in anhydrous acetone, and 0.73 g of methanesulfonyl isocyanate is added thereto at room temperature. After the mixture is stirred for 30 minutes, the mixture is concentrated under reduced pressure to remove solvent. The residue is collected by filtration, and washed with water and ether, successively. The crude product thus obtained is recrystallized from a mixture of acetone and ether. 1.56 g of N-methanesulfonyl-2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazollidine-3-carboxamide are obtained.

後処理

  1. customat room temperature
  2. concentrationthe mixture is concentrated under reduced pressure
  3. customto remove solvent
  4. filtrationThe residue is collected by filtration
  5. washwashed with water and ether
  6. customThe crude product thus obtained
  7. customis recrystallized from a mixture of acetone and ether

出典と根拠

ORDレコード
ord-4309e47a359d4d8aa7980c2c2a42a140
出典データセット
uspto-grants-1987_08
特許番号
US04689327

反応ノート

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