Triethylamine → HCID 13079701、化合物

HRID 1703101ノート

反応式

HRID 1703101 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH2:17][OH:18])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>ClCCl>[CH3:26][S:27]([O:18][CH2:17][CH2:16][CH2:15][C:12]1[CH:11]=[CH:10][C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:14][CH:13]=1)(=[O:29])=[O:28]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 27640763-(4-(Benzyloxy)phenyl)propan-1-ol

生成物 1

HCID 13079701HCID 13079701、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-10 °C

実験手順

To a solution of 11.0 g. of 3-[p-(benzyloxy)phenyl]propanol and 10.4 ml. of triethylamine in 175 ml. of dichloromethane chilled to -10° C. is added dropwise, over 10 minutes, a solution of 3.89 ml. of methanesulfonyl chloride in 10 ml. of dichloromethane. The solution is stirred at -10° C. for 30 minutes, washed with 150 ml. of cold water, 75 ml. of cold 10% HCl, 75 ml. of cold saturated sodium bicarbonate, 75 ml. of cold saturated sodium chloride solution and dried over magnesium sulfate. The solvent is removed in vacuo to give off-white crystals, m.p. 65°-69° C.

後処理

  1. additionis added dropwise, over 10 minutes
  2. washwashed with 150 ml
  3. dry with materialof cold saturated sodium chloride solution and dried over magnesium sulfate
  4. customThe solvent is removed in vacuo
  5. customto give off-white crystals, m.p. 65°-69° C.

出典と根拠

ORDレコード
ord-6ae58c997ae64fbca6bed664343072b0
出典データセット
uspto-grants-1982_09
特許番号
US04350822

反応ノート

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