Disodium 2,3-dihydroxybutanedioate → HCID 86698315, 화합물

HRID 1050281노트

반응식

HRID 1050281 반응식
[N:1]([C@H:4]1[CH2:9][C@H:8]2[C@H:10]3[C@H:19]([CH2:20][CH2:21][C@:6]2([CH3:7])[CH2:5]1)[C:18]1[CH:17]=[CH:16][C:15]([O:22][CH3:23])=[CH:14][C:13]=1[CH2:12][CH2:11]3)=[N+]=[N-].[H-].[Al+3].[Li+].[H-].[H-].[H-].CCOCC.O.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[Na+]>C1COCC1>[NH2:1][C@H:4]1[CH2:9][C@H:8]2[C@H:10]3[C@H:19]([CH2:20][CH2:21][C@:6]2([CH3:7])[CH2:5]1)[C:18]1[CH:17]=[CH:16][C:15]([O:22][CH3:23])=[CH:14][C:13]=1[CH2:12][CH2:11]3

참가 물질

6

반응물 4

HCID 13355Disodium 2,3-dihydroxybutanedioateHCID 21226445Aluminium lithium hydrideHCID 21584184Diethylether waterHCID 86698314HCID 86698314, 화합물

생성물 1

HCID 86698315HCID 86698315, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirred solution of 1.28 g (4.1 mmol) 16β-azido-3-methoxy-estra-1,3,5(10)-triene in 30 ml abs. THF, 10 ml of a 1M lithium aluminum hydride solution in THF (Fluka) is added dropwise under cooling. The mixture is stirred for further 30 min at RT, followed by cautious addition of ether/water at 0° C. and subsequent addition of sodium tartrate solution. After three subsequent extractions of the aqueous phase with ether, the combined organic phases are washed twice with water, dried with sodium sulfate and concentrated. Yield after recrystallization from hexane: 1.05 g (89%), white solid matter with F=90-94° C.

후처리

  1. temperatureunder cooling
  2. extractionAfter three subsequent extractions of the aqueous phase with ether
  3. washthe combined organic phases are washed twice with water
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated
  6. customYield
  7. customafter recrystallization from hexane
  8. customwith F=90-94° C.

출처 및 근거

ORD 기록
ord-dba318140d62484a97d94b8b5b60f423
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09382288B2

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