Methanol → HCID 20155099、化合物

HRID 364916

反応式

HRID 364916 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 20155099HCID 20155099、化合物

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9eba8f1869a947b2b8374ea56de86b98
出典データセット
uspto-grants-1986_08
特許番号
US04607006

関連ノート

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