Tetrahydrofuran → HCID 20284789、化合物

HRID 127520

反応式

HRID 127520 の反応式
[CH3:1][NH:2][CH2:3][CH:4]1[C:16]2C3C(=CC=CC=3)N[C:8]=2[S:7]CC1.C([N:19]([CH2:22][CH3:23])[CH2:20][CH3:21])C.[C:24]([O:28][C:29](SC1N=C(C)C=C(C)N=1)=[O:30])([CH3:27])([CH3:26])[CH3:25].O1[CH2:44][CH2:43][CH2:42][CH2:41]1>>[C:24]([O:28][C:29]([N:2]([CH2:3][CH:4]1[C:23]2[C:21]3[C:20](=[CH:41][CH:42]=[CH:43][CH:44]=3)[NH:19][C:22]=2[S:7][CH2:8][CH2:16]1)[CH3:1])=[O:30])([CH3:27])([CH3:26])[CH3:25]

参加物

5

反応物 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 148428O-(1,1-Dimethylethyl) S-(4,6-dimethyl-2-pyrimidinyl) carbonothioateHCID 30560964-Methylaminomethyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole

生成物 1

HCID 20284789HCID 20284789、化合物収率 93%

実験手順

To a solution of 4-methylaminomethyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole (4.41 g) in tetrahydrofuran (50 ml) are added triethylamine (4 ml) and 2-(t-butoxycarbonylthio)-4,6-dimethylpyrimidine (4.76 l g) successively at room temperature. The mixture is stirred at room temperature for 2.5 hours and evaporated to remove the solvent. The residue is extracted with chloroform after addition of water. The extract is washed, dried and evaporated to give crude crystals. Recrystallization from acetone gives the title compound (5.57 g) melting at 220°-222° C. (decomp.).

後処理

  1. customevaporated
  2. customto remove the solvent
  3. extractionThe residue is extracted with chloroform
  4. additionafter addition of water
  5. washThe extract is washed
  6. customdried
  7. customevaporated
  8. customto give crude crystals
  9. customRecrystallization from acetone

出典と根拠

ORDレコード
ord-769f2ca02fde48049ef46625e6e97232
出典データセット
uspto-grants-1981_03
特許番号
US04256640

関連ノート

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