Trifluoroacetic acid → HCID 66714093、化合物

HRID 2173764ノート

反応式

HRID 2173764 の反応式
[N:1]1([CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][C:18]([O:20]C(C)(C)C)=[O:19])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[N:1]1([CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][C:18]([OH:20])=[O:19])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 66716176HCID 66716176、化合物

生成物 1

HCID 66714093HCID 66714093、化合物収率 99%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1 g of tert-butyl 3-{2-[2-(2-morpholin-4-yl-ethoxy)-ethoxy]-ethoxy}-propanoate in 50 ml of DCM was added 4 ml of TFA. The mixture was stirred for 10 hours at room temperature and then concentrated under reduced pressure and purified on a Mega BE-SCX, 25GM 150ML cartridge (Varian), using washing with MeOH and detachment of the expected product with a 2N solution of ammonia in MeOH. The fractions containing the desired product were combined and concentrated under reduced pressure. 830 mg of 3-{2-[2-(2-morpholin-4-yl-ethoxy)-ethoxy]-ethoxy}-propanoic acid were obtained. LC/MS (E): tr (ELSD)=0.16 min; [M+H]+: m/z 292

後処理

  1. concentrationconcentrated under reduced pressure
  2. custompurified on a Mega BE-SCX, 25GM 150ML cartridge (Varian)
  3. washusing washing with MeOH and detachment of the expected product with a 2N solution of ammonia in MeOH
  4. additionThe fractions containing the desired product
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-34f9624ce5e64cbbb4ef9bb13ec151a5
出典データセット
uspto-grants-2015_06
特許番号
US09056914B2

反応ノート

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