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Triethylamine → (2-Methylcarbamoyl-6-oxo-5,6-dihydro-1H-[1,2]diazepino[4,5,6-cd]indol-8-yl)-carbamic acid tert-butyl ester

HRID 1064174
ノート
印刷プレビュー

反応式

HRID 1064174 の反応式
Cl.CN.C[O:5][C:6]([C:8]1[NH:9][C:10]2[CH:11]=[C:12]([NH:22][C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH:13]=[C:14]3[C:20](=[O:21])[NH:19][N:18]=[CH:17][C:16]=1[C:15]=23)=O.[CH2:30]([N:32](CC)CC)C>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].CO>[C:26]([O:25][C:23](=[O:24])[NH:22][C:12]1[CH:13]=[C:14]2[C:20](=[O:21])[NH:19][N:18]=[CH:17][C:16]3=[C:8]([C:6](=[O:5])[NH:32][CH3:30])[NH:9][C:10]([CH:11]=1)=[C:15]23)([CH3:28])([CH3:27])[CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 6364545Methylamine hydrochloride2 回HCID 1361816128-tert-Butoxycarbonylamino-6-oxo-5,6-dihydro-1H-[1,2]diazepino[4,5,6-cd]indole-2-carboxylic acid methyl ester

生成物 1

HCID 136181651(2-Methylcarbamoyl-6-oxo-5,6-dihydro-1H-[1,2]diazepino[4,5,6-cd]indol-8-yl)-carbamic acid tert-butyl ester収率 29.1%

試薬・触媒・溶媒 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 887Methanol溶媒

実験手順

Preparation of example 161 was carried out in a manner analogous to step 5 of Example 147, except that methylamine hydrochloride was substituted for methanol. Thus CO was bubbled through a mixture of Intermediate 147(d) from Example 147 (200 mg, 0.529 mmol), triethylamine (0.29 mL, 2.11 mmol), methylamine hydrochloride (71 mg, 1.06 mmol), and 1,1′-bis(diphenylphosphino)ferrocenedichloropalladium (II) (86 mg, 0.106 mmol). Reaction conditions, work up and silica gel chromatography (eluted with 46:4:25 dichloromethane: methanol: ethyl acetate) were also carried out in an analogous manner and afforded the title compound (55 mg, 0.154 mmol) in 29% yield.

後処理

  1. customPreparation of example 161
  2. customReaction conditions
  3. washsilica gel chromatography (eluted with 46:4:25 dichloromethane: methanol: ethyl acetate)

出典と根拠

ORDレコード
ord-a4df4d984cfb42a09cee87ae823cb609
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06967198B2

反応ノート

読み込み中…

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