Benzylamine → HCID 54426674、化合物

HRID 865613ノート

反応式

HRID 865613 の反応式
[O:1]1[CH2:20][CH:2]1[CH2:3][O:4][CH2:5][CH2:6][CH2:7][Si:8]([CH3:19])([O:14][Si:15]([CH3:18])([CH3:17])[CH3:16])[O:9][Si:10]([CH3:13])([CH3:12])[CH3:11].[CH2:21]([NH2:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(O)(C)C>[CH2:21]([NH:28][CH2:20][CH:2]([OH:1])[CH2:3][O:4][CH2:5][CH2:6][CH2:7][Si:8]([CH3:19])([O:14][Si:15]([CH3:18])([CH3:17])[CH3:16])[O:9][Si:10]([CH3:13])([CH3:12])[CH3:11])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

参加物

4

反応物 2

HCID 7504BenzylamineHCID 62635Trisiloxane, 1,1,1,3,5,5,5-heptamethyl-3-(3-(2-oxiranylmethoxy)propyl)-2 回

生成物 1

HCID 54426674HCID 54426674、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

反応条件

温度
80 °C

実験手順

A 500-ml, three-necked, round-bottomed flask equipped with a stirrer, addition funnel, and condenser was charged with 100 g (0.30 mole) of the epoxy trisiloxane (Compound I) of Example 1 dissolved in 200 ml of isopropanol. The addition funnel was charged with a solution of 42.8 g (0.4 mole) of benzylamine (Aldrich) in 100 ml of isopropanol; the solution was added drop-wise to the flask contents at room temperature. The resulting reaction solution was heated at 80° C. for eight hours, after which time the solvent was removed under reduced pressure using a rotary evaporator. The residue, an oil, was passed through a short silica column using 10% ethyl acetate in hexane as eluent. The yield of Compound V, a colorless oil, was 127.8 g (97%). The following elemental analysis was obtained:

後処理

  1. customA 500-ml, three-necked, round-bottomed flask equipped with a stirrer, addition funnel, and condenser
  2. additionthe solution was added drop-wise to the flask contents at room temperature
  3. customThe resulting reaction solution
  4. customafter which time the solvent was removed under reduced pressure
  5. customa rotary evaporator
  6. customThe following elemental analysis was obtained

出典と根拠

ORDレコード
ord-421cfe939bc84f5cb7eb371e11a63fce
出典データセット
uspto-grants-1996_10
特許番号
US05567372

反応ノート

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