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Lithium borohydride → Ether isohexane

HRID 2388770
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HRID 2388770 반응식
[CH2:1]([O:3][C:4](=O)[C@H:5](OC1C=C(NS(C2N=CN(C)C=2)(=O)=O)N=C(S[CH2:25][C:26]2[CH:31]=C[CH:29]=[C:28](F)[C:27]=2F)N=1)C)[CH3:2].[BH4-].[Li+]>C1COCC1>[CH3:2][CH2:1][O:3][CH2:4][CH3:5].[CH3:29][CH2:28][CH2:27][CH:26]([CH3:31])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4148881Lithium borohydrideHCID 536283532-[[2-[[(2,3-difluorophenyl)methyl]thio]-6-[[(1-methyl-1H-imidazol-4-yl)sulfonyl]amino]-4-pyrimidinyl]oxy]-(2R)-propanoic acid ethyl ester

생성물 1

HCID 21882825Ether isohexane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The title compound was prepared according to the procedure outlined in example 24 using 2-[[2-[[(2,3-difluorophenyl)methyl]thio]-6-[[(1-methyl-1H-imidazol-4-yl)sulfonyl]amino]-4-pyrimidinyl]oxy]-(2R)-propanoic acid ethyl ester (the product of step i) (0.28 g), THF (8 mL) and 2 M lithium borohydride in THF (0.81 mL). Purification was by reverse phase HPLC (symmetry as the stationary phase and TFA/acetonitrile as the mobile phase). The resulting oil was triturated with toluene, methanol, then ether/iso-hexane to give the title compound as a white solid. Yield: 0.12 g

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후처리

  1. customThe title compound was prepared
  2. customPurification
  3. customThe resulting oil was triturated with toluene, methanol

출처 및 근거

ORD 기록
ord-aa02024bbc0047e081b4f897f068d36d
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08269002B2

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