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Hydrochloric Acid → HCID 58679133, 화합물

HRID 18943
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HRID 18943 반응식
[Cl:1][C:2]1[C:10]2[O:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][C:3]=1[NH2:11].Cl.[O:13]1CCOC[CH2:14]1.C(Cl)(Cl)=O>C1COCC1>[Cl:1][C:2]1[C:10]2[O:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][C:3]=1[N:11]=[C:14]=[O:13]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6371PhosgeneHCID 312751,4-DioxaneHCID 58679182HCID 58679182, 화합물

생성물 1

HCID 58679133HCID 58679133, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
70 °C

실험 절차

To a vial containing 4-chlorobenzo[d][1,3]dioxol-5-amine (28.8 mg, 0.168 mmol, 1 equiv.) in 1 mL THF was added 4M HCl in 1,4-dioxane (0.042 mL, 1 equiv.) followed by phosgene (20% in toluene; 0.360 mL, 0.684 mmol, 4 equiv.). The vial was capped and heated to 70° C. for 1 h, the solvent was removed under, the residue redissolved in toluene and solvent was again removed under vacuum to eliminate any remaining phosgene yielding 4-chloro-5-isocyanatobenzo[d][1,3]dioxole used as such in the next step.

후처리

  1. customThe vial was capped
  2. customthe solvent was removed under, the residue
  3. dissolutionredissolved in toluene
  4. customsolvent was again removed under vacuum

출처 및 근거

ORD 기록
ord-dd6ff86954744922a24da377a7d58ba8
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07741479B2

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