Chloroform → 4-[(4,5-Dihydro-2-thiazolyl)amino]tetrahydro-3,5-bis(phenylmethylene)-2H-pyran-4-ol

HRID 65670

반응식

HRID 65670 반응식
[NH2:1][C:2]1[S:3][CH2:4][CH2:5][N:6]=1.[C:7]1([CH:13]=[C:14]2[C:19](=[O:20])[C:18](=[CH:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:17][O:16][CH2:15]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(Cl)(Cl)Cl>CC(C)=O>[S:3]1[CH2:4][CH2:5][N:6]=[C:2]1[NH:1][C:19]1([OH:20])[C:18](=[CH:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:17][O:16][CH2:15][C:14]1=[CH:13][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 156894,5-Dihydro-2-thiazolamineHCID 286335tetrahydro-3,5-bis(phenylmethylene)-4H-pyran-4-one

생성물 1

HCID 541285554-[(4,5-Dihydro-2-thiazolyl)amino]tetrahydro-3,5-bis(phenylmethylene)-2H-pyran-4-ol수율 45.5%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A solution of 2-amino-2-thiazoline (2.2 g, 22 mmole) in 100 ml of acetone is added to a suspension of tetrahydro-3,5-bis(phenylmethylene)-4H-pyran-4-one (5.0 g, 18 mmole) in 50 ml of acetone and heated at reflux temperature for 5 hours and then kept at room temperature overnight. Chloroform (75 ml) is added to the stirred mixture and, after 10 minutes, the product is collected and washed with acetone to give 3.1 g of crude product. When the filtrate, concentrated and resuspended in acetone, is stirred with additional 2-amino-2-thiazoline (2.2 g) at room temperature overnight, another 2.5 g is isolated for a combined yield of 5.6 g (82%).

후처리

  1. temperatureheated
  2. temperatureat reflux temperature for 5 hours
  3. customthe product is collected
  4. washwashed with acetone

출처 및 근거

ORD 기록
ord-719a7ddb9172448c83f5f21cbf1ee683
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128648

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