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Phenyl isocyanate → HCID 67297600, 화합물

HRID 629018
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인쇄 미리보기

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HRID 629018 반응식
[CH3:1][S:2][C:3]1[C:4]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[N:5][C:6]([C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=2)=[N:7][CH:8]=1.[C:22]1([N:28]=[C:29]=[O:30])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>CN(C=O)C.C1COCC1>[CH3:1][S:2][C:3]1[C:4]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[N:5][C:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:29]([NH:28][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[O:30])=[CH:11][CH:10]=2)=[N:7][CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7672Phenyl isocyanateHCID 67295403HCID 67295403, 화합물

생성물 1

HCID 67297600HCID 67297600, 화합물수율 30.4%

시약·촉매·용매 1

HCID 21974620tetrahydrofuran N,N-dimethylformamide용매

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온도
80 °C

실험 절차

A mixture of 4-(5-(methylthio)-4-morpholinopyrimidin-2-yl)benzeneamine (0.1 g, 0.33 mmole), co-solvent (5 ml, DMF/THF=6/40) and phenyl isocyanate (0.2 ml, 0.92 mmole) was heated to 80° C. After 12 hrs, the reaction mixture was cooled, and the THF removed in vacuo. Then the mixture was diluted with EA, washed with brine, and dried (MgSO4). The solvent was removed in vacuo. Purification of the residue on silica gel (EA/Hex=1/2) yielded the desired compound (42.2 mg, 30.4%).

후처리

  1. temperaturethe reaction mixture was cooled
  2. customthe THF removed in vacuo
  3. additionThen the mixture was diluted with EA
  4. washwashed with brine
  5. dry with materialdried (MgSO4)
  6. customThe solvent was removed in vacuo
  7. customPurification of the residue on silica gel (EA/Hex=1/2)

출처 및 근거

ORD 기록
ord-cdbdc5a0a9c74437a56a44475a3b42ae
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315491B2

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