Water → [((1R, 2R)-2-Aminocyclohexyl]amino}-2,5,6-trichloro-1,3-dicyanobenzene

HRID 1744710

반응식

HRID 1744710 반응식
[Cl:1][C:2]1[C:7]([C:8]#[N:9])=[C:6](Cl)[C:5]([Cl:11])=[C:4]([Cl:12])[C:3]=1[C:13]#[N:14].C(N(CC)CC)C.[CH2:22]1[CH2:27][C@@H:26]([NH2:28])[C@H:25]([NH2:29])[CH2:24][CH2:23]1.O>CC#N>[NH2:28][C@@H:26]1[CH2:27][CH2:22][CH2:23][CH2:24][C@H:25]1[NH:29][C:6]1[C:5]([Cl:11])=[C:4]([Cl:12])[C:3]([C:13]#[N:14])=[C:2]([Cl:1])[C:7]=1[C:8]#[N:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 15910ChlorothalonilHCID 438061,2-Diaminocyclohexane, trans-

생성물 1

HCID 86593704[((1R, 2R)-2-Aminocyclohexyl]amino}-2,5,6-trichloro-1,3-dicyanobenzene수율 89.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To the suspension of 2,4,5,6-tetrachloro-1,3-dicyanobenzene (2.0 g, 7.52 mmol) and triethylamine (5 ml) in methyl cyanide (40 ml) is added a solution of (1R,2R)-diaminocyclohexane (0.85 g, 7.52 mmol) in methyl cyanide (10 ml). The mixture is mixed for 60 min. at 120° C., then cooled to room temperature and the water (10 ml) is slowly added. After cooling in a refrigerator the solid is recovered on a G4 filter and washed with water-methyl cyanide (1:1) and with methyl cyanide. Finally, the product is vacuum-dried on KOH tablets. 2.32 g (89%) of pale yellow powder are obtained, dec. at a temp. greater than 190° C.

후처리

  1. additionThe mixture is mixed for 60 min. at 120° C.
  2. temperatureAfter cooling in a refrigerator the solid
  3. customis recovered on a G4
  4. filtrationfilter
  5. washwashed with water-methyl cyanide (1:1) and with methyl cyanide
  6. customFinally, the product is vacuum-dried on KOH tablets

출처 및 근거

ORD 기록
ord-7aff9991f246471f932297b63437d2cc
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07018537B2

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