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Triphosgene → HCID 11484465, 화합물

HRID 1760838
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HRID 1760838 반응식
[CH2:1]([NH:6][C:7]1[CH:16]=[CH:15][C:14]2[C:13]([CH3:18])([CH3:17])[CH2:12][CH2:11][C:10]([CH3:20])([CH3:19])[C:9]=2[CH:8]=1)[CH2:2][CH2:3][CH2:4][CH3:5].[Cl:21][C:22](Cl)([O:24]C(=O)OC(Cl)(Cl)Cl)Cl>C1COCC1>[CH2:1]([N:6]([C:7]1[CH:16]=[CH:15][C:14]2[C:13]([CH3:18])([CH3:17])[CH2:12][CH2:11][C:10]([CH3:19])([CH3:20])[C:9]=2[CH:8]=1)[C:22]([Cl:21])=[O:24])[CH2:2][CH2:3][CH2:4][CH3:5]
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참가 물질

4

반응물 2

HCID 94429TriphosgeneHCID 11208062HCID 11208062, 화합물

생성물 1

HCID 11484465HCID 11484465, 화합물수율 292.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of pentyl-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-amine (33) (1.0 g, 3.6 mmole) in 20 mL of THF was treated with 380 mg of triphosgene (0.35 eq.). The reaction mixture was stirred at reflux for three hours, poured onto 30 mL ice-water and extracted with three portions of 30 mL of ethyl acetate. The combined organic extracts were dried over MgSO4, filtered and concentrated in vacuo to give 1.26 g of pentyl-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-carbamoyl chloride (35) as a white solid, which was used without purification.

후처리

  1. temperatureat reflux for three hours
  2. extractionextracted with three portions of 30 mL of ethyl acetate
  3. dry with materialThe combined organic extracts were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-19fe911379794f8989a19ce623b95a1e
출처 데이터셋
uspto-grants-2005_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06844466B2

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