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Trifluoroacetic acid methylene chloride → (S)-N-ethyl-N-(morpholin-3-ylmethyl)ethanamine hydrochloride salt

HRID 1771207
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HRID 1771207 반응식
[CH2:1]([N:3]([CH2:6][C@H:7]1[CH2:12][O:11][CH2:10][CH2:9][N:8]1C(OC(C)(C)C)=O)[CH2:4][CH3:5])[CH3:2].C(O)(C(F)(F)F)=O.C(Cl)[Cl:28]>>[ClH:28].[CH2:1]([N:3]([CH2:6][C@H:7]1[CH2:12][O:11][CH2:10][CH2:9][NH:8]1)[CH2:4][CH3:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 21863450Trifluoroacetic acid methylene chlorideHCID 66723823(S)-tert-butyl 3-((diethylamino)methyl)morpholine-4-carboxylate2회

생성물 1

HCID 66723589(S)-N-ethyl-N-(morpholin-3-ylmethyl)ethanamine hydrochloride salt수율 67%

실험 절차

(S)-tert-butyl 3-((diethylamino)methyl)morpholine-4-carboxylate (INTERMEDIATE 86, STEP 1) was dissolved with TFA/DCM, (10 ml, 1:1 v/v) and the resulting mixture was stirred for 1 hour at room temperature. The volatiles were removed under reduced pressure and the concentrate was treated with 4N HCl in dioxane (5 ml), stirred for 10 minutes and the volatiles were removed under reduced pressure. The resulting semi solid was triturated with diethyl ether (2×30 ml), filtered and dried to give the title product (0.65 g, yield: 67%).

후처리

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  • customThe volatiles were removed under reduced pressure
  • additionthe concentrate was treated with 4N HCl in dioxane (5 ml)
  • stirringstirred for 10 minutes
  • customthe volatiles were removed under reduced pressure
  • customThe resulting semi solid was triturated with diethyl ether (2×30 ml)
  • filtrationfiltered
  • customdried
  • 출처 및 근거

    ORD 기록
    ord-7e6e43db23fb4e7294d5c52eac9d5f22
    출처 데이터셋
    uspto-grants-2016_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09248140B2

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