Butyl isocyanate → HCID 14727326、化合物

HRID 1284929ノート

反応式

HRID 1284929 の反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:4]=[C:5]([CH:18]=[CH:19][CH:20]=1)[C:6]([CH2:16][CH3:17])([OH:15])[C:7]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][C:8]=1[OH:14].[CH2:23]([N:27]=[C:28]=[O:29])[CH2:24][CH2:25][CH3:26]>CN(C)C1C=CN=CC=1.ClCCl>[F:1][C:2]([F:21])([F:22])[C:3]1[CH:4]=[C:5]([CH:18]=[CH:19][CH:20]=1)[C:6]([CH2:16][CH3:17])([OH:15])[C:7]1[CH:12]=[CH:11][C:10]([O:13][C:28](=[O:29])[NH:27][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:9][C:8]=1[O:14][C:28](=[O:29])[NH:27][CH2:23][CH2:24][CH2:25][CH3:26]

参加物

5

反応物 2

HCID 8110Butyl isocyanateHCID 14009067HCID 14009067、化合物

生成物 1

HCID 14727326HCID 14727326、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

6.2 g. of 3-trifluoromethyl-2',4'-dihydroxy-α-ethyl-benzhydrol, 4.4 g. of butyl isocyanate and 0.06 g. of 4-dimethylamino-pyridine in 40 ml. of dichloromethane are refluxed for 60 minutes. The reaction mixture is cooled down, and the organic phase is extracted with a 5% aqueous potassium hydroxide solution and washed to neutral with water. The organic phase is dried over anhydrous magnesium sulfate, filtered and solvent is distilled off under reduced pressure. Crystallization of the residue from toluene yields 8.7 g. of the end product, which melts at 110° to 111° C.

後処理

  1. temperatureThe reaction mixture is cooled down
  2. extractionthe organic phase is extracted with a 5% aqueous potassium hydroxide solution
  3. washwashed to neutral with water
  4. dry with materialThe organic phase is dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. distillationsolvent is distilled off under reduced pressure
  7. customCrystallization of the residue from toluene
  8. customyields 8.7 g

出典と根拠

ORDレコード
ord-2612b681e0de46c582075db2191e22a1
出典データセット
uspto-grants-1986_01
特許番号
US04564630

反応ノート

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