Tetrahydrofuran → HCID 20284789, 화합물

HRID 127520

반응식

HRID 127520 반응식
[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]

참가 물질

5

반응물 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

생성물 1

HCID 20284789HCID 20284789, 화합물수율 93%

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-769f2ca02fde48049ef46625e6e97232
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256640

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