Triethylamine → HCID 20539557, 화합물

HRID 1065633

반응식

HRID 1065633 반응식
[C:1]1([C:7]2[CH:25]=[CH:24][C:10]([O:11][CH:12]([N:19]3[CH:23]=[N:22][CH:21]=[N:20]3)[CH:13]([OH:18])[C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:26]([Si:28]([CH2:32][CH3:33])([CH2:30][CH3:31])Cl)[CH3:27].C(N(CC)CC)C>C1COCC1.CN(C)C1C=CN=CC=1>[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([O:11][CH:12]([N:19]3[CH:23]=[N:22][CH:21]=[N:20]3)[CH:13]([O:18][Si:28]([CH2:32][CH3:33])([CH2:30][CH3:31])[CH2:26][CH3:27])[C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:24][CH:25]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 13819ChlorotriethylsilaneHCID 91656Bitertanol

생성물 1

HCID 20539557HCID 20539557, 화합물수율 40.7%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매

반응 조건

온도
45 °C

실험 절차

5.5 g of 1-p-phenylphenoxy-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol is dissolved in 25 ml of THF. 2.9 g of triethylchlorosilane and 0.2 g of 4-dimethylaminopyridine are added under a nitrogen blanket. The mixture is heated to 45° C., and 3.3 g of triethylamine is added in portions. After the mixture has been stirred for 14 hours at from 40° to 50° C. it is cooled to room temperature, undissolved matter is filtered off, and the filtrate is concentrated. The product is further purified either by adding petroleum ether, followed by filtration and concentration, or by gel filtration (SiO2, CHCl3). There is obtained 3 g of 1-p-phenylphenoxy-3,3-dimethyl-2-triethylsiloxy-1-(1,2,4-triazol-1-yl)-butane.

후처리

  1. temperatureis cooled to room temperature
  2. filtrationundissolved matter is filtered off
  3. concentrationthe filtrate is concentrated
  4. customThe product is further purified either
  5. additionby adding petroleum ether
  6. filtrationfollowed by filtration and concentration
  7. filtrationby gel filtration (SiO2, CHCl3)

출처 및 근거

ORD 기록
ord-2f9a22956e5947f0a32bdb954971dfd7
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04330535

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