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Ammonia → HCID 58413407, 화합물

HRID 532276
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HRID 532276 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][CH:10]([O:12][C:13]1[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=1[NH:20][C:21]1[C:22]2[C:29]([CH3:30])=[C:28]([C:31](O)=[O:32])[S:27][C:23]=2[N:24]=[CH:25][N:26]=1)[CH3:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].C[N:35](C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C(N(CC)CC)C.N>CN(C=O)C>[C:31]([C:28]1[S:27][C:23]2[N:24]=[CH:25][N:26]=[C:21]([NH:20][C:14]3[CH:15]=[CH:16][C:17]([F:19])=[CH:18][C:13]=3[O:12][CH:10]([CH3:11])[CH2:9][NH:8][C:6](=[O:7])[O:5][C:1]([CH3:2])([CH3:4])[CH3:3])[C:22]=2[C:29]=1[CH3:30])(=[O:32])[NH2:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 58413372HCID 58413372, 화합물

생성물 1

HCID 58413407HCID 58413407, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

4-(2-(1-(tert-Butoxycarbonylamino)propan-2-yloxy)-4-fluorophenylamino)-5-methyl-thieno[2,3-d]pyrimidine-6-carboxylic acid (250 mg) and TBTU (170 mg) was dissolved in DMF (3 ml) and triethylamine (1900) was added. The mixture was stirred at room temperature for 10 min, then 0.5 ml conc. ammonia was added. The reaction was stirred for 2 h. Then the reaction mixture was concentrated in vacuo and purified by RP-chromatography (water with 0.2% trifluoroacetic acid/methanol 72-100%) to give the title compound.

후처리

  1. stirringThe reaction was stirred for 2 h
  2. concentrationThen the reaction mixture was concentrated in vacuo
  3. custompurified by RP-chromatography (water with 0.2% trifluoroacetic acid/methanol 72-100%)

출처 및 근거

ORD 기록
ord-5f5fdb4f717a456ba5800e619850974c
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853193B2

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