Hydrochloric Acid → 3-Amino-propionic acid dipropylcarbamoylmethyl ester

HRID 2170102ノート

反応式

HRID 2170102 の反応式
[CH2:1]([N:4]([CH2:24][CH2:25][CH3:26])[C:5]([CH2:7][O:8][C:9](=[O:23])[CH2:10][CH2:11][NH:12]C(OCC1C=CC=CC=1)=O)=[O:6])[CH2:2][CH3:3].Cl>O1CCOCC1>[CH2:24]([N:4]([CH2:1][CH2:2][CH3:3])[C:5]([CH2:7][O:8][C:9](=[O:23])[CH2:10][CH2:11][NH2:12])=[O:6])[CH2:25][CH3:26]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 667979022-(Dipropylamino)-2-oxoethyl 3-(((benzyloxy)carbonyl)amino)propanoate

生成物 1

HCID 866633473-Amino-propionic acid dipropylcarbamoylmethyl ester

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a cooled stirred solution of 3-tert-butoxycarbonylamino-propionic acid dipropylcarbamoylmethyl ester (step 1) (36.5 g, 110 mmol) in dry dioxane under N2 was added dropwise 4N HCl in dioxane (18.12 ml, 597 mmol). The resulting mixture was allowed to warm to RT and stirred overnight. The solvent was removed in vacuo and the crude product was suspended in EtOAc (500 ml) and sonicated for 1 h. The resulting white precipitate was isolated by filtration and was dried under vacuum at 40° C. for 1 h to afford a pale yellow solid. Recrystallisation from EtOAc afforded the title compound; LC-MS Rt 0.77 mins; 231.2 [M+H]+, Method 2minLC_v003.

後処理

  1. customThe solvent was removed in vacuo
  2. customsonicated for 1 h
  3. customThe resulting white precipitate was isolated by filtration
  4. customwas dried under vacuum at 40° C. for 1 h
  5. customto afford a pale yellow solid
  6. customRecrystallisation from EtOAc

出典と根拠

ORDレコード
ord-85d22566204240469af7eb265ea7cde2
出典データセット
uspto-grants-2015_06
特許番号
US09050339B2

反応ノート

読み込み中…