Methanol → 9-Ethyl-3-isocyanatocarbazole

HRID 2413673

反応式

HRID 2413673 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 201550999-Ethyl-3-isocyanatocarbazole

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 in 500 ml of ethyl acetate, and cooled to precipitate and then filter off solids. The filtrate was concentrated 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 in 500 ml of ethyl acetate
  6. temperaturecooled
  7. customto precipitate
  8. filtrationfilter off solids
  9. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-9e5e9b55f683429fa89f2bf67ac707ea
出典データセット
uspto-grants-1988_01
特許番号
US04719174

関連ノート

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