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4-Methylmorpholine → HCID 86761673, 화합물

HRID 1875330
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HRID 1875330 반응식
[CH3:1][N:2]1[CH2:11][CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:12]([OH:14])=O)[CH:8]=2)[CH2:3]1.CN1CCOCC1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH:46]1[CH2:50][CH2:49][C@@H:48]([NH:51][C:52](=[O:58])[O:53][C:54]([CH3:57])([CH3:56])[CH3:55])[CH2:47]1>CN(C=O)C>[CH3:1][N:2]1[CH2:11][CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:12]([N:46]3[CH2:50][CH2:49][C@@H:48]([NH:51][C:52](=[O:58])[O:53][C:54]([CH3:56])([CH3:55])[CH3:57])[CH2:47]3)=[O:14])[CH:8]=2)[CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 79724-MethylmorpholineHCID 1514397(3R)-(+)-3-(tert-Butoxycarbonylamino)pyrrolidineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 57423969HCID 57423969, 화합물

생성물 1

HCID 86761673HCID 86761673, 화합물

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

1.1 g (4.8 mmol) 2-methyl-1,2,3,4-tetrahydroisoquinoline-6-carboxylic acid (as hydrochloride) are dissolved in 12 ml DMF, mixed with 2.1 ml (19.3 mmol) NMM and 1.8 g (4.8 mmol) HATU and stirred for five minutes at RT. Then 0.9 g (4.8 mmol) tert. Butyl (R)-pyrrolidin-3-yl-carbamate are added and the mixture is stirred for 16 hours. Then the mixture is poured onto water and extracted with DCM. The organic phase is separated using a phase separation cartridge and evaporated to dryness i. vac. The residue is purified by flash chromatography on silica gel (eluant DCM/MeOH 9:1 to 8:2).

후처리

  1. stirringthe mixture is stirred for 16 hours
  2. additionThen the mixture is poured onto water
  3. extractionextracted with DCM
  4. customThe organic phase is separated
  5. customa phase separation cartridge
  6. customevaporated to dryness i
  7. customThe residue is purified by flash chromatography on silica gel (eluant DCM/MeOH 9:1 to 8:2)

출처 및 근거

ORD 기록
ord-2f1e97eb315640ac84214f719f63568b
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08309542B2

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