Sodium borohydride → HCID 67348945, 화합물

HRID 1916338노트

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HRID 1916338 반응식
[O:1]=[C:2]1[N:6]([C:7]2[CH:8]=[CH:9][C:10]3[S:15][CH2:14][C:13](=[O:16])[NH:12][C:11]=3[CH:17]=2)[CH2:5][C@@H:4]([CH2:18][CH2:19][CH2:20][NH:21][C@H:22]2[C:32]3[C:33]4[N:24]([C:25](=[O:34])[CH:26]=[N:27][C:28]=4[CH:29]=[CH:30][CH:31]=3)[CH2:23]2)[O:3]1.[BH4-].[Na+]>CO.ClCCCl>[O:1]=[C:2]1[N:6]([C:7]2[CH:8]=[CH:9][C:10]3[S:15][CH2:14][C:13](=[O:16])[NH:12][C:11]=3[CH:17]=2)[CH2:5][C@@H:4]([CH2:18][CH2:19][CH2:20][NH:21][C@H:22]2[C:32]3[C:33]4[N:24]([C:25](=[O:34])[CH2:26][NH:27][C:28]=4[CH:29]=[CH:30][CH:31]=3)[CH2:23]2)[O:3]1

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 45380794HCID 45380794, 화합물

생성물 1

HCID 67348945HCID 67348945, 화합물수율 78%

시약·촉매·용매 1

HCID 22134543HCID 22134543, 화합물용매

실험 절차

A solution of the compound of Example 48 (33 mg) in MeOH/DCE (5 mL; 4:1) was treated with NaBH4 (3 mg) for 30 min then quenched with 1M. HCl (1 mL) and partitioned between DCM and an aq. NH4OH solution. The org. layer was washed with water and brine, dried over MgSO4 and purified by CC (EA/MeOH 19:1 to 9:1 containing 1% NH4OH) affording a colourless solid (26 mg; 78% yield).

후처리

  1. customthen quenched with 1M
  2. customHCl (1 mL) and partitioned between DCM
  3. washlayer was washed with water and brine
  4. dry with materialdried over MgSO4
  5. custompurified by CC (EA/MeOH 19:1 to 9:1 containing 1% NH4OH)
  6. customaffording a colourless solid (26 mg; 78% yield)

출처 및 근거

ORD 기록
ord-d5d8a1cadd864919a89e07b583a1d38c
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618092B2

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