Methanol → HCID 20155099, 화합물

HRID 364916

반응식

HRID 364916 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH2:15][CH3:16])[C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3.C(N(CC)CC)C.[CH3:24][OH:25].C1(N=C=NC2CCCCC2)CCCCC1>C(=S)=S>[CH2:15]([N:6]1[C:5]2[CH:4]=[CH:3][C:2]([N:1]=[C:24]=[O:25])=[CH:14][C:13]=2[C:12]2[C:7]1=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH3:16]

참가 물질

6

반응물 4

HCID 887MethanolHCID 8471TriethylamineHCID 85883-Amino-9-ethylcarbazoleHCID 10868Dicyclohexylcarbodiimide

생성물 1

HCID 20155099HCID 20155099, 화합물

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

38.6 g of 3-amino-9-ethylcarbazole and 27.9 ml of triethylamine were added to 300 ml of methanol, and, while cooling with ice, 15.2 g of carbon disulfide was added dropwise thereto. After conducting reaction at room temperature for 3 hours, 41.3 g of dicyclohexylcarbodiimide was added thereto, followed by reacting at room temperature for 4 hours. Crystals thus precipitated were collected by filtration, heat-refluxed for 10 minutes in 500 ml of ethyl acetate, and cooled to precipitate and then filter off solids. The filtrate was concentrated by removing solvents in vacuo to obtain the desired product (29 g).

후처리

  1. additionwas added dropwise
  2. customreaction at room temperature for 3 hours
  3. customCrystals thus precipitated
  4. filtrationwere collected by filtration
  5. temperatureheat-refluxed for 10 minutes in 500 ml of ethyl acetate
  6. temperaturecooled
  7. customto precipitate
  8. filtrationfilter off solids
  9. concentrationThe filtrate was concentrated
  10. customby removing solvents in vacuo

출처 및 근거

ORD 기록
ord-9eba8f1869a947b2b8374ea56de86b98
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04607006

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