Isobutyl isothiocyanate → trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-N'-(2-methylpropyl)thiourea

HRID 16160

반응식

HRID 16160 반응식
[CH2:1]([N:5]=[C:6]=[S:7])[CH:2]([CH3:4])[CH3:3].[Cl:8][C:9]1[CH:28]=[CH:27][C:12]2[O:13][C:14]3[CH:26]=[CH:25][CH:24]=[CH:23][C:15]=3[C@@H:16]3[C@H:21]([NH2:22])[CH2:20][CH2:19][CH2:18][N:17]3[C:11]=2[CH:10]=1>C1COCC1>[Cl:8][C:9]1[CH:28]=[CH:27][C:12]2[O:13][C:14]3[CH:26]=[CH:25][CH:24]=[CH:23][C:15]=3[C@@H:16]3[C@H:21]([NH:22][C:6]([NH:5][CH2:1][CH:2]([CH3:4])[CH3:3])=[S:7])[CH2:20][CH2:19][CH2:18][N:17]3[C:11]=2[CH:10]=1

참가 물질

4

반응물 2

HCID 68960Isobutyl isothiocyanateHCID 70883458trans-7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine

생성물 1

HCID 86599868trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-N'-(2-methylpropyl)thiourea수율 12%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Isobutyl isothiocyanate (3.35 mg, 0.03 mmol) was added to trans-7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (5 mg, 0.02 mmol) in 1 mL of THF. The resulting mixture was stirred at room temperature for 18 h. The mixture was evaporated under reduced pressure. Crystallisation from methanol gave trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-N′-(2-methylpropyl)thiourea (1 mg, 12%). Data: (m/z)=416 (M+H)+.

후처리

  1. customThe mixture was evaporated under reduced pressure
  2. customCrystallisation from methanol

출처 및 근거

ORD 기록
ord-1d851d7ba4c147f5b6c7b8ee51973cf0
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737136B2

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