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Tetrahydrofuran → HCID 824395, 화합물

HRID 1045380
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HRID 1045380 반응식
[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=O.CCN(C(C)C)C(C)C.CN(C(O[N:28]1[N:36]=N[C:30]2C=CC=C[C:29]1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C1C[O:45]CC1>>[C:29]([NH:28][NH:36][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][CH:10]=[C:2]([I:1])[CH:3]=1)(=[O:45])[CH3:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 8028TetrahydrofuranHCID 120603-Iodobenzoic acidHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate

생성물 1

HCID 824395HCID 824395, 화합물

실험 절차

To a suspension of 3-iodobenzoic acid (2.0 g, 8.06 mmol) in 60 ml of THF there are added, in succession, DIPEA (1.83 ml, 10.48 mmol) and TBTU (2.59 g, 8.06 mmol). The reaction mixture is stirred overnight at ambient temperature. 1.19 g (16.12 mmol) of acetyl hydrazide are added and the reaction mixture is heated at reflux for 30 hours. After evaporation to dryness, the residue is taken up in water with a small amount of CH2Cl2; a thick precipitate forms, which is filtered off to yield the expected product.

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후처리

  1. temperaturethe reaction mixture is heated
  2. temperatureat reflux for 30 hours
  3. customAfter evaporation to dryness
  4. filtrationa thick precipitate forms, which is filtered off

출처 및 근거

ORD 기록
ord-30e15cc75a064ee5bba6b0e58eec69b0
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08569285B2

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