Triethylamine → HCID 20539557、化合物

HRID 1065633

反応式

HRID 1065633 の反応式
[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

参加物

6

反応物 3

HCID 8471TriethylamineHCID 13819ChlorotriethylsilaneHCID 91656Bitertanol

生成物 1

HCID 20539557HCID 20539557、化合物収率 40.7%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
45 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2f9a22956e5947f0a32bdb954971dfd7
出典データセット
uspto-grants-1982_05
特許番号
US04330535

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