Butyl isocyanate → HCID 14727326, 화합물

HRID 1284929노트

반응식

HRID 1284929 반응식
[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]

참가 물질

5

반응물 2

HCID 8110Butyl isocyanateHCID 14009067HCID 14009067, 화합물

생성물 1

HCID 14727326HCID 14727326, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2612b681e0de46c582075db2191e22a1
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04564630

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