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Ammonium Chloride → HCID 71270118, 화합물

HRID 927110
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HRID 927110 반응식
[CH2:1]([O:8][C:9]1[N:10]=[N:11][C:12]([C:23]#[CH:24])=[CH:13][C:14]=1[O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([Li])CCC.[O:30]1[CH2:35][CH2:34][C:33](=[O:36])[CH2:32][CH2:31]1.[Cl-].[NH4+]>O1CCCC1>[CH2:16]([O:15][C:14]1[CH:13]=[C:12]([C:23]#[C:24][C:33]2([OH:36])[CH2:34][CH2:35][O:30][CH2:31][CH2:32]2)[N:11]=[N:10][C:9]=1[O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 121599Tetrahydro-4H-pyran-4-oneHCID 866770253,4-Bis(benzyloxy)-6-ethynylpyridazine2회HCID 178418339Butyllithium

생성물 1

HCID 71270118HCID 71270118, 화합물수율 501%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

3,4-bis(Benzyloxy)-6-ethynylpyridazine (Intermediate 5; 3.0 g, 9.49 mmol) was dissolved in tetrahydrofuran (24 ml) under nitrogen atmosphere and the resulting solution was cooled to −78° C. n-Butyl lithium (23% solution in hexane; 7.92 ml, 28.48 mmol, 3.0 eq) was added slowly at −78° C., and the resulting mixture was allowed to stir for 30 minutes. Dihydro-2H-pyran-4(3H)-one (1.0 g, 10.44 mmol, 1.1 equiv.) was added slowly to reaction mass and the whole was allowed to warm to room temperature. The crude mixture was then poured into a saturated solution of aqueous ammonium chloride (300 ml) and product was extracted into ethyl acetate (100 ml×2). The organic layer was separated, washed with brine, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography on silica gel (eluting with 0-30% ethyl acetate in hexane) to yield the desired material (2.0 g, 501% yield).

후처리

  1. additionwas added slowly at −78° C.
  2. extractionwas extracted into ethyl acetate (100 ml×2)
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by column chromatography on silica gel (eluting with 0-30% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-bb9d9ca9d41a4df7836d51eb2c26467e
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290456B2

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