Formaldehyde → HCID 21481152, 화합물

HRID 435646노트

반응식

HRID 435646 반응식
N[C:2]1[CH:30]=[CH:29][C:5]2[S:6][C:7]3[CH:28]=[CH:27][CH:26]=[CH:25][C:8]=3[CH:9]([N:11]3[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][N:19]4[CH2:23][CH2:22][O:21][C:20]4=[O:24])[CH2:13][CH2:12]3)[CH2:10][C:4]=2[CH:3]=1.C=O.[C:33](#N)C.[C:36]([BH3-])#[N:37].[Na+]>C(O)(=O)C>[CH3:33][N:37]([CH3:36])[C:2]1[CH:30]=[CH:29][C:5]2[S:6][C:7]3[CH:28]=[CH:27][CH:26]=[CH:25][C:8]=3[CH:9]([N:11]3[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][N:19]4[CH2:23][CH2:22][O:21][C:20]4=[O:24])[CH2:13][CH2:12]3)[CH2:10][C:4]=2[CH:3]=1

참가 물질

6

반응물 4

HCID 712FormaldehydeHCID 6342AcetonitrileHCID 5003444Sodium cyanoborohydrideHCID 21481150HCID 21481150, 화합물

생성물 1

HCID 21481152HCID 21481152, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

7 g of 3-[2-[4-(2-amino-10,11-dihydro-dibenzo[b,f]-thiepin-10-yl)-1-piperazinyl]-ethyl]-2-oxazolidinone, 13.1 ml of 40% formaldehyde and 61 ml of acetonitrile are treated with 3.32 of sodium cyanoborohydride and the resulting mixture is treated dropwise over period of 10 minutes with 1.5 ml of acetic acid. The mixture is stirred for a further 90 minutes, treated dropwise with a further 1.5 ml of acetic acid and again stirred for 15 minutes. The mixture is now extracted with 200 ml of ether and the organic phase washed three times with 1-N aqueous potassium hydroxide solution, dried over sodium sulphate and evaporated. There is obtained 3-[2-[4-(10,11-dihydro-2-dimethylamino-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl]-2-oxazolidinone which melts at 168°-170° C. After recrystallisation from ethanol, this compound melts at 171°-173° C. By treatment with maleic acid there is obtained the corresponding maleate which melts at 143.5°-144.5° C after recrystallisation from acetonitrile.

후처리

  1. stirringagain stirred for 15 minutes
  2. extractionThe mixture is now extracted with 200 ml of ether
  3. washthe organic phase washed three times with 1-N aqueous potassium hydroxide solution
  4. dry with materialdried over sodium sulphate
  5. customevaporated

출처 및 근거

ORD 기록
ord-3b5e72521f244ed2b6f59067f3049aa2
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04006145

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