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Diisopropylcarbodiimide → HCID 178473461, 화합물

HRID 968234
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HRID 968234 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[N:16]=[C:15]([NH2:17])[C:14]([NH2:18])=[C:13]([NH2:19])[N:12]=1.[CH2:20]([O:22][C:23]([N:25]=[C:26]=S)=[O:24])[CH3:21].C(N=C=NC(C)C)(C)C>C(#N)C.C(N(CC)CC)C>[NH2:19][C:13]1[N:12]=[C:11]([S:10][CH2:9][C:3]2[CH:4]=[CH:5][CH:6]=[C:7]([F:8])[C:2]=2[F:1])[N:16]=[C:15]2[C:14]=1[N:18]=[C:26]([NH:25][C:23](=[O:24])[O:22][CH2:20][CH3:21])[NH:17]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 12734DiisopropylcarbodiimideHCID 85320Ethyl isothiocyanatoformateHCID 222885032-[[(2,3-Difluorophenyl)methyl]thio]-4,5,6-pyrimidinetriamine

생성물 1

HCID 178473461HCID 178473461, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매2회HCID 8471Triethylamine
용매

실험 절차

A solution of the product of example 5, step (c) (10.5 g) in acetonitrile (50 ml) and triethylamine (17 ml) was added to an ice cold stirred solution of ethoxycarbonylisothiocyanate (3 ml) in acetonitrile (50 ml). This mixture was then stirred at room temperature for 20 min. Diisopropylcarbodiimide (4.5 ml) was then added and the reaction mixture was stirred at reflux for 2 hr and allowed to cool. The reaction mixture was evaporated to dryness and purified by flash chromatography on silica gel (ethyl acetate:dichloromethane, 1:1) to yield the sub-titled compound as a yellow solid (3.0 g).

후처리

  1. stirringthe reaction mixture was stirred
  2. temperatureat reflux for 2 hr
  3. temperatureto cool
  4. customThe reaction mixture was evaporated to dryness
  5. custompurified by flash chromatography on silica gel (ethyl acetate:dichloromethane, 1:1)

출처 및 근거

ORD 기록
ord-aff72cbdeaa648a788c164f18094cde2
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06958344B2

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