Triethylamine → HCID 23134071、化合物

HRID 416520

反応式

HRID 416520 の反応式
[C:1]([O:5][C:6](=[O:12])[NH:7][CH2:8][CH:9]([OH:11])[CH3:10])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22]>ClCCl>[C:1]([O:5][C:6]([NH:7][CH2:8][CH:9]([O:11][S:21]([CH3:20])(=[O:23])=[O:22])[CH3:10])=[O:12])([CH3:2])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 9920508tert-butyl N-(2-hydroxypropyl)carbamate

生成物 1

HCID 23134071HCID 23134071、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

8.24 g (47.0 mmol) (2-Hydroxy-propyl)-carbamic acid tert-butyl ester were dissolved in 100 ml dichloromethane. 7.8 ml (1.2 equiv.) triethylamine were added and the mixture was cooled to 0° C. At that temperature 4.37 ml (1.2 equiv.) methanesulfonyl chloride were added dropwise. The resulting solution was allowed to reach room temperature and stirred for further 4 h. The mixture was diluted with 100 ml dichloromethane and washed sequentially with a 5% KHSO4-solution, water and brine. The organic phase was dried over anhydrous MgSO4 and concentrated under reduced pressure to give methanesulfonic acid 2-tert-butoxycarbonylamino-1-methyl-ethyl ester in crude form as yellow oil.

後処理

  1. customto reach room temperature
  2. washwashed sequentially with a 5% KHSO4-solution, water and brine
  3. dry with materialThe organic phase was dried over anhydrous MgSO4
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-449167024039450ea1bd024540009d2a
出典データセット
uspto-grants-2012_01
特許番号
US08088925B2

関連ノート

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