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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → (3beta,5beta,7alpha,12alpha)-3-(1-Oxopent-4-enyl)amino-7,12-dihydroxy-cholan-24-oic acid methyl ester

HRID 266024
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HRID 266024 반응식
[C:1](O)(=[O:6])[CH2:2][CH2:3][CH:4]=[CH2:5].C(N(CC)CC)C.ClC(OCC(C)C)=O.[CH3:23][O:24][C:25](=[O:52])[CH2:26][CH2:27][C@H:28]([C@@H:30]1[C@:47]2([CH3:48])[C@H:33]([C@H:34]3[C@H:44]([CH2:45][C@@H:46]2[OH:49])[C@:42]2([CH3:43])[C@@H:37]([CH2:38][C@@H:39]([NH2:50])[CH2:40][CH2:41]2)[CH2:36][C@H:35]3[OH:51])[CH2:32][CH2:31]1)[CH3:29]>C1COCC1>[CH3:23][O:24][C:25](=[O:52])[CH2:26][CH2:27][C@H:28]([C@@H:30]1[C@:47]2([CH3:48])[C@H:33]([C@H:34]3[C@H:44]([CH2:45][C@@H:46]2[OH:49])[C@:42]2([CH3:43])[C@@H:37]([CH2:38][C@@H:39]([NH:50][C:1](=[O:6])[CH2:2][CH2:3][CH:4]=[CH2:5])[CH2:40][CH2:41]2)[CH2:36][C@H:35]3[OH:51])[CH2:32][CH2:31]1)[CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 611384-Pentenoic acidHCID 62365Isobutyl chloroformateHCID 10364902HCID 10364902, 화합물

생성물 1

HCID 54437505(3beta,5beta,7alpha,12alpha)-3-(1-Oxopent-4-enyl)amino-7,12-dihydroxy-cholan-24-oic acid methyl ester

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

A solution of 4-pentenoic acid (marketed product) and triethylamine in THF was added drop by drop, under nitrogen and at 5° C., to isobutyl chloroformate and subsequently with a solution of (3β,5β,7α,12α)-3-amino-7,12-dihydroxy-cholan-24-oic acid methyl ester (prepared according to the procedure described in EXAMPLE 5) in THF. When the reaction was over, solvent was evaporated and the residue was taken up with H2O and AcOEt. The organic phase was separated, washed with H2O, dried over Na2SO4 and evaporated under reduced pressure. The residue was purified by flash chromatography to obtain the desired product.

후처리

  1. customwas evaporated
  2. customThe organic phase was separated
  3. washwashed with H2O
  4. dry with materialdried over Na2SO4
  5. customevaporated under reduced pressure
  6. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-348cfa841ead497595c808489a63437d
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05649537

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