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Methyl chloroformate → HCID 68486281, 화합물

HRID 1891210
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HRID 1891210 반응식
[F:1][C:2]1[C:3]([O:28][CH2:29][C:30]2[CH:35]=[CH:34][C:33]([CH:36]3[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]3)=[CH:32][CH:31]=2)=[C:4]([C:8]2[N:13]=[C:12]([N:14]3[C:18]([C:19]([F:22])([F:21])[F:20])=[C:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:16]=[N:15]3)[CH:11]=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1.C(N(C(C)C)CC)(C)C.Cl[C:52]([O:54][CH3:55])=[O:53]>C(Cl)Cl.C([O-])(O)=O.[Na+]>[CH2:26]([O:25][C:23]([C:17]1[CH:16]=[N:15][N:14]([C:12]2[N:13]=[C:8]([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[C:3]=3[O:28][CH2:29][C:30]3[CH:31]=[CH:32][C:33]([CH:36]4[CH2:41][CH2:40][N:39]([C:52]([O:54][CH3:55])=[O:53])[CH2:38][CH2:37]4)=[CH:34][CH:35]=3)[CH:9]=[CH:10][CH:11]=2)[C:18]=1[C:19]([F:21])([F:22])[F:20])=[O:24])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6586Methyl chloroformateHCID 81531DiisopropylethylamineHCID 68486762HCID 68486762, 화합물

생성물 1

HCID 68486281HCID 68486281, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 516892Sodium Bicarbonate용매

실험 절차

To a solution of the title compound from Example 5 Step C (194 mg, 0.34 mmol) in DCM (2 mL) were added diisopropyl ethyl amine (0.60 mL, 3.41 mmol) and methyl chloroformate (0.08 mL, 1.02 mmol). The reaction mixture was stirred for 1 h at ambient temperature, then was diluted with sat. aq. NaHCO3 and extracted with DCM. The organic phase was separated, dried over sodium sulfate, filtered, and concentrated in vacuo. The product was used in the subsequent step without further purification: LCMS m/z 626.9 [M+H]+.

후처리

  1. extractionextracted with DCM
  2. customThe organic phase was separated
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe product was used in the subsequent step without further purification

출처 및 근거

ORD 기록
ord-547b99ae05c444bbad9f7117b88f940f
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507512B2

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