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Lithocholic Acid → Cholanic acid

HRID 618606
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HRID 618606 반응식
[CH3:1][C@@H:2]([C@@H:8]1[C@@:12]2([CH3:27])[CH2:13][CH2:14][C@@H:15]3[C@@:20]4([CH3:26])[CH2:21][CH2:22][C@@H:23](O)[CH2:24][C@H:19]4[CH2:18][CH2:17][C@H:16]3[C@@H:11]2[CH2:10][CH2:9]1)[CH2:3][CH2:4][C:5]([OH:7])=[O:6]>C(OC(=O)C)(=O)C>[C:5]([OH:7])(=[O:6])[CH2:4][CH2:3][C@H:2]([C@@H:8]1[C@:12]2([CH3:27])[C@H:11]([C@H:16]3[C@H:15]([CH2:14][CH2:13]2)[C@:20]2([CH3:26])[CH:19]([CH2:24][CH2:23][CH2:22][CH2:21]2)[CH2:18][CH2:17]3)[CH2:10][CH2:9]1)[CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 9903Lithocholic Acid

생성물 1

HCID 9548797Cholanic acid수율 50%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

A solution of 1 g of the lithocholic acid dimer prepared by the inventors, viz. bis(5(-cholan-24-oic-3(-yl) sebacate, in 6 ml of acetic anhydride was heated to 120° C. in an oil bath for 1 h. The solvent was partially removed and the mixed anhydride prepolymer was allowed to crystallize at -10° C. The product was filtered out, washed with a small amount of cold acetic anhydride and dried under vacuum at room temperature for two days. The requested bis (5(-cholan-24-oic acid 3(-yl) sebacate prepolymer (PreLCA) was obtained with a yield of 50%.

후처리

  1. customThe solvent was partially removed
custom
to crystallize at -10° C
  • filtrationThe product was filtered out
  • washwashed with a small amount of cold acetic anhydride
  • customdried under vacuum at room temperature for two days
  • 출처 및 근거

    ORD 기록
    ord-796cbf678a554efea7d9dda6f7169654
    출처 데이터셋
    uspto-grants-1999_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05955068

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