Toluene → 4-Isocyanato-5,6,7,8-tetrahydronaphthalene-1-carbonitrile

HRID 501512

반응식

HRID 501512 반응식
Cl.[NH2:2][C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[C:6]([C:13]#[N:14])=[CH:5][CH:4]=1.[C:15]([O-])(O)=[O:16].[Na+].C(Cl)(Cl)=O.C1(C)C=CC=CC=1>C(Cl)Cl>[N:2]([C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[C:6]([C:13]#[N:14])=[CH:5][CH:4]=1)=[C:15]=[O:16]

참가 물질

6

반응물 4

HCID 1140TolueneHCID 6371PhosgeneHCID 516892Sodium BicarbonateHCID 1317269774-Amino-5,6,7,8-tetrahydronaphthalene-1-carbonitrile, hydrochloride salt

생성물 1

HCID 597543044-Isocyanato-5,6,7,8-tetrahydronaphthalene-1-carbonitrile수율 99.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

To a stirring suspension of compound 2D (0.10 g, 0.48 mmol) and NaHCO3 (0.404 g, 4.80 mmol) in CH2Cl2 (4 mL) cooled to 0° C. was rapidly added a solution of phosgene (20%) in toluene (0.95 mL, 4.32 mmol). After addition, the mixture was stirred at rt for 2 h, then filtered to remove the solid. The filtrate was concentrated under reduced pressure, the resulting solid residue dried under vacuum for 1 h to afford compound 2E (95 mg) as a light yellow solid.

후처리

  1. additionAfter addition
  2. filtrationfiltered
  3. customto remove the solid
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe resulting solid residue dried under vacuum for 1 h

출처 및 근거

ORD 기록
ord-d93fd10229394289bffabb38e613fd6d
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772267B2

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